Description:FORM 2
THE PATENTS ACT 1970
(39 of 1970)
&
The Patent Rules 2003
COMPLETE SPECIFICATION
(see sections 10 & rule 13)
1. TITLE OF THE INVENTION
“A PROCESS FOR PREPARING DERIVATIVE(S) OF AMMONIUM PERCHLORATE (ND4ClO4)”
2. APPLICANT (S)
NAME NATIONALITY ADDRESS
CLEARSYNTH LABS LIMITED Indian 17th Floor, Lotus Nilkamal Business Park, New Link Road, Andheri [West], Mumbai - 400053, Maharashtra, India.
3. PREAMBLE TO THE DESCRIPTION

COMPLETE SPECIFICATION
The following specification particularly describes the invention and the manner in which it is to be performed

FIELD OF INVENTION
The present invention relates to derivative of ammonium perchlorate and preparation process and use thereof. Most particularly, it relates a process for preparing deuterated ammonium perchlorate (ND₄ClO₄). The prepared deuterated compound has wide application various high-energy applications.

BACKGROUND OF INVENTION
Ammonium Perchlorate (AP) is an essential component in various high-energy applications, particularly as a powerful oxidizer in solid rocket propellants, explosives, and pyrotechnics. Its widespread usage stems from its ability to provide the oxygen necessary for combustion, making it indispensable in propellant formulations. Despite its advantages, AP presents several challenges and limitations that can impact its efficiency, safety, and environmental sustainability. These challenges primarily revolve around issues such as thermal stability, decomposition kinetics, environmental concerns, and limitations in spectroscopic studies.
AP is prone to thermal decomposition when exposed to elevated temperatures, which significantly affects its stability. The decomposition process of AP is highly exothermic, meaning it releases a substantial amount of energy. This exothermic nature can lead to thermal runaway reactions, especially in storage or handling under harsh environmental conditions. Such reactions pose severe safety risks, reducing the margin for safe handling and increasing the potential for accidents in both industrial and laboratory settings.
The kinetics of AP decomposition are often too rapid for applications requiring controlled combustion. The fast reaction rate can lead to inefficiencies in energy utilization and, in some cases, uncontrolled reactions. These limitations restrict its utility in applications where precise modulation of thrust or energy release is critical, such as in advanced propulsion systems.
Perchlorate ions, a by-product of AP decomposition, are environmentally persistent and have a significant potential for contamination of soil and water. These ions pose serious health risks to humans and ecosystems when not adequately managed. Their long-term persistence also increases the regulatory challenges associated with the use, storage, and disposal of AP, adding complexity to its application in environmentally sensitive areas.
The rapid decomposition and interaction dynamics of AP create difficulties in detailed spectroscopic studies. The hydrogen vibrations and proton transfer processes associated with AP are complex and challenging to analyze using conventional methods. This limits the understanding of its combustion mechanisms, making it difficult to optimize formulations for improved performance or safety.
Deuterated Ammonium Perchlorate (DAP), denoted as ND₄ClO₄, is a modified form of AP where the hydrogen atoms are replaced with deuterium.
This isotopic substitution brings about significant improvements in addressing the challenges associated with standard AP, leveraging the unique properties of deuterium to enhance performance, safety, and environmental sustainability.
One of the most notable advantages of DAP is its enhanced thermal stability. The replacement of hydrogen with deuterium increases the bond dissociation energy of N-D bonds compared to N-H bonds. This leads to a slower rate of thermal decomposition, making DAP more stable under high-temperature conditions. The improved stability ensures safer handling and storage, particularly in extreme environments where thermal sensitivity is a concern. This characteristic is especially valuable in long-term storage and transportation of solid propellants.
The isotopic substitution in DAP introduces a kinetic isotope effect, which slows down the reaction rate of its decomposition. This slower reaction rate allows for better control over the combustion process, leading to more efficient and predictable energy release. Such control is crucial in solid rocket propellants and pyrotechnics, where precision and safety are paramount. By modulating the reaction kinetics, DAP enhances the overall performance and reliability of these systems.
The slower decomposition and improved combustion efficiency of DAP result in a significant reduction in the formation of perchlorate residues. This minimizes the environmental footprint of DAP compared to standard AP, addressing one of the most critical concerns associated with its use. By reducing soil and water contamination risks, DAP supports compliance with stringent environmental regulations and promotes sustainable practices in industries reliant on high-energy oxidizers.
The presence of deuterium in DAP alters its vibrational frequencies, simplifying the analysis of decomposition pathways and interaction dynamics. This makes it a valuable tool for spectroscopic studies, enabling researchers to gain deeper insights into the mechanisms of combustion and decomposition. Such insights can drive the development of advanced oxidizer formulations and improve the safety and efficiency of existing systems.
Henceforth, there is a need to develop a process for preparing ammonium-d4 perchlorate to overcome the forementioned problems.
Thus, the present invention provides a transformative solution to the challenges posed by standard Ammonium Perchlorate. Its enhanced thermal stability, controlled reaction kinetics, reduced environmental impact, and utility in advanced spectroscopic studies make it an ideal choice for applications demanding precision, safety, and sustainability. By leveraging the unique properties of deuterium, Ammonium-d4 perchlorate not only addresses existing limitations but also opens new avenues for innovation in the fields of propulsion, pyrotechnics, and environmental chemistry.

OBJECTS OF THE INVENTION
The main object of the present invention is to provide a process for preparing deuterated ammonium perchlorate (ND₄ClO₄).
Another object of the present invention is to provide characterisation of the prepared deuterated ammonium perchlorate (ND₄ClO₄).
Another object of the present invention is to study the effects of isotopic substitution on the combustion behaviour of ammonium perchlorate, which is a common oxidizer in solid rocket propellants.
Another object of the present invention is to prepare Ammonium-d4 perchlorate which has low cost, high deuteration rate and simple preparation and easy operation.
Yet another object of the present invention is to use in the chemical reaction studies to trace reaction mechanisms involving deuterium atoms.
Yet another embodiment of the present invention is to serve deuterated ammonium perchlorate as a reference compound for understanding deuterium's impact on vibrational and NMR spectroscopy.

SUMMARY OF THE INVENTION
Main aspect of the present invention provides a process for preparing deuterated ammonium perchlorate (ND4ClO4), the process comprising:
a) making a mixture comprising ammonium perchlorate and a solvent;
b) heating the mixture and maintaining at the same temperature to obtain a reaction mass;
c) isolating the deuterated ammonium perchlorate (ND₄ClO₄) from the reaction mass to obtain an isolated deuterated ammonium perchlorate (ND₄ClO₄); and
d) drying the isolated deuterated ammonium perchlorate (ND₄ClO₄) to obtain deuterated ammonium perchlorate (ND₄ClO₄) which having IP 95% to 98%.

DETAILED DESCRIPTION OF THE INVENTION
In the specification, different terms are used to describes the invention. The definitions of the terms are provided below.
The term ‘derivative(s) of ammonium perchlorate’ or ‘deuterated ammonium perchlorate’ or ‘ammonium-d4 perchlorate’ used herein means hydrogen atoms in the ammonium ion (NH₄⁺) are replaced with deuterium (²H or D). The terms ‘derivatives of ammonium perchlorate’ and ‘deuterated ammonium’ and ‘ammonium-d4 perchlorate’ can be written as ND₄ClO₄ and used interchangeably in the specification.
The term ‘reaction mass’ used herein refers to the combined mass obtained after completion of reaction which includes solvent, product (deuterated ammonium perchlorate) and/or any by-product.
The term ‘isolating the deuterated ammonium perchlorate (ND₄ClO₄)’ used herein refers to obtaining the deuterated ammonium perchlorate (ND₄ClO₄) from reaction mass by work-up. It may involve a series of steps such as but are not limited to extraction, precipitation, crystallization, recrystallisation, acid-base treatment, neutralization and combinations thereof.
The term ‘solvent’ used herein refers to a substance, typically a liquid, in which other substances (solutes) are dissolved to form a solution. The solvent used to carry out the present invention can be polar or nonpolar solvent. The said solvent may be used in hydrous and/or anhydrous form.
The solvent may include such as but is not limited to water, acid, ketone, ester, hydrocarbon, ethers, alcohols, amides, deuterated form of above-mentioned solvent(s).
One of the embodiments of the present invention provides a process for preparing deuterated ammonium perchlorate (ND₄ClO₄), the process comprising:
a) making a mixture comprising ammonium perchlorate and a solvent;
b) heating the mixture and maintaining at the same temperature to obtain a reaction mass;
c) isolating the deuterated ammonium perchlorate (ND₄ClO₄) from the reaction mass to obtain an isolated deuterated ammonium perchlorate (ND₄ClO₄); and
d) drying the isolated deuterated ammonium perchlorate (ND₄ClO₄) to obtain deuterated ammonium perchlorate (ND₄ClO₄) which having IP 95% to 98%.
Another embodiment of the present invention provides a process for preparing deuterated ammonium perchlorate (ND₄ClO₄), wherein the making a mixture comprising ammonium perchlorate and a solvent is carried out at a temperature in the range of 10oC to 25oC.
Another embodiment of the present invention provides a process for preparing ammonium-d4 perchlorate, wherein heating the mixture and maintaining at the same temperature to obtain a reaction mass is carried out at a temperature in the range of 20oC to 35oC for a time period in the range of 10hrs to 14hrs.
Another embodiment of the present invention provides a process for preparing deuterated ammonium perchlorate (ND₄ClO₄), wherein isolating the deuterated ammonium perchlorate (ND₄ClO₄) from the reaction mass to obtain isolated deuterated ammonium perchlorate (ND₄ClO₄) is carried out by distilling the solvent under vacuum at a temperature in the range of 20oC to 35oC.
Another embodiment of the present invention provides a process for preparing deuterated ammonium perchlorate (ND₄ClO₄), wherein drying the isolated deuterated ammonium perchlorate (ND₄ClO₄) to obtain deuterated ammonium perchlorate (ND₄ClO₄) which having IP 95-98% is carried out under vacuum.
Another embodiment of the present invention provides a process for preparing ammonium-d4 perchlorate (ND₄ClO₄), wherein solvent is selected from wherein solvent is selected from water, alcohols, ethers, ketones, acids, esters, acetonitrile (ACN), halogenated solvent(s) and/or deuterated form of water, alcohols, ethers, ketones, acids, esters, and/or deuterated halogenated solvent(s).
Another embodiment of the present invention provides a process for preparing deuterated ammonium perchlorate (ND₄ClO₄), wherein the solvent is deuterated water (D2O).
Another embodiment of the present invention provides a process for preparing deuterated ammonium perchlorate (ND4ClO4), wherein the process is carried out for 1cycle to 5 cycles, preferably 3 cycles.
Another embodiment of the present invention provides a process for preparing deuterated ammonium perchlorate (ND4ClO4), wherein in the deuterated compound, preferably at least 40% by weight of the hydrogen atoms are deuterium atoms.
Another embodiment of the present invention provides a process for preparing deuterated ammonium perchlorate (ND4ClO4), wherein proposed to use deuterated ammonium perchlorate (ND4ClO4) as fuels and/or oxidizing agents, alternatively also as binders, for pyrotechnic IR active compositions.
Another embodiment of the present invention provides a process for preparing deuterated ammonium perchlorate, wherein the prepared deuterate ammonium perchlorate may further be purified any known conventional methods.
In another embodiment of the present invention there is provided a process for preparing deuterated ammonium perchlorate (ND₄ClO₄), wherein said process is carried out or represented by following way.
Scheme:

Advantages of the present invention:
1. The present invention provides an improved thermal stability ammonium-d4 perchlorate
2. The replacement of hydrogen with deuterium increases the bond dissociation energy of N-D bonds compared to N-H bonds. This leads to slower thermal decomposition, enhancing the stability of the compound.
3. The isotopic substitution reduces the reaction rate due to the kinetic isotope effect. This provides better control over the combustion process, resulting in more efficient and predictable energy release.
4. The slower decomposition and better combustion efficiency of DAP reduce the formation of perchlorate residues, mitigating environmental contamination.
5. Supports compliance with environmental regulations and reduces long-term ecological risks.
6. The presence of deuterium alters the vibrational frequencies, making it easier to study decomposition pathways and interactions.
7. The present invention provides insights into improving formulations and developing advanced oxidizers.
8. The present invention is carried out at lower temperature therefore reduced formation of impurities or by-products.
9. The deuterated solvent used in the present invention is easily recovered and recycle for continuous production of deuterated ammonium perchlorate.
The examples provided in the definitions present in this application are non-inclusive unless otherwise stated. They include but are not limited to the recited examples.
Example
1. Preparation of Ammonium-d4 perchlorate (ND₄ClO₄):
In a 500ml RBF 100g of unlabelled ammonium perchlorate was taken followed by addition D2O 500 ml at temperature 20oC- 25oC. The resulting mixture was gradually heated up to 25oC-30oC and maintained the same temperature for 12 hrs. The D2O was distilled under vacuum at 25oC-30oC. The solid obtained was dried under vacuum to get white powder of ammonium-d4 perchlorate with IP 95-98%.

We claim:
1. A process for preparing deuterated ammonium perchlorate (ND₄ClO₄), the process comprising:
a) making a mixture comprising ammonium perchlorate and a solvent;
b) heating the mixture and maintaining at the same temperature to obtain a reaction mass;
c) isolating the deuterated ammonium perchlorate (ND₄ClO₄) from the reaction mass to obtain an isolated deuterated ammonium perchlorate (ND₄ClO₄); and
d) drying the isolated deuterated ammonium perchlorate (ND₄ClO₄) to obtain deuterated ammonium perchlorate (ND₄ClO₄) which having IP 95% to 98%.
2. The process as claimed in claim 1, wherein the making a mixture comprising ammonium perchlorate and a solvent is carried out at a temperature in the range of 10oC to 25oC.
3. The process as claimed in claim 1, wherein heating the mixture and maintaining the same temperature to obtain a reaction mass is carried out at a temperature in the range of 20oC to 35oC for a time period in the range of 10 hrs to 14 hrs.
4. The process as claimed in claim 1, wherein isolating the deuterated ammonium perchlorate (ND₄ClO₄) from the reaction mass to obtain isolated deuterated ammonium perchlorate (ND₄ClO₄) is carried out by distilling the solvent under vacuum at a temperature in the range of 20oC to 35oC.
5. The process as claimed in claim 1, wherein drying the isolated deuterated ammonium perchlorate (ND₄ClO₄) to obtain deuterated ammonium perchlorate (ND₄ClO₄) which having IP 95-98% is carried out under vacuum.
6. The process as claimed in claim 1, wherein solvent is selected from water, alcohols, ethers, ketones, acids, esters, acetonitrile (ACN), halogenated solvent(s) and/or deuterated form of water, alcohols, ethers, ketones, acids, esters, and/or deuterated halogenated solvent(s).
7. The process as claimed in claim 5, wherein the solvent is deuterated water (D2O).

Dated this: 23rd day of January 2025

Vijaykumar Shivpuje
IN/PA-1096
Agent for the Applicant

To
The Controller of Patents,
The Patent Office, Mumbai

ABSTRACT

“A PROCESS FOR PREPARING DERIVATIVE(S) OF AMMONIUM PERCHLORATE (ND4ClO4)”

The present invention provides derivative(s) of ammonium perchlorate and preparation method and use thereof. Most particularly, it relates a process for preparing deuterated ammonium perchlorate (ND₄ClO₄). The said process is carried out by: (a) making a mixture comprising ammonium perchlorate and a solvent; (b) heating the mixture and maintaining the same temperature to obtain a reaction mass; (c) isolating the deuterated ammonium perchlorate (ND₄ClO₄) from the reaction mass to obtain an isolated deuterated ammonium perchlorate (ND₄ClO₄); and (d) drying the isolated deuterated ammonium perchlorate (ND₄ClO₄) to obtain deuterated ammonium perchlorate (ND₄ClO₄) with IP 95-98%.

, Claims:We claim:
1. A process for preparing deuterated ammonium perchlorate (ND₄ClO₄), the process comprising:
a) making a mixture comprising ammonium perchlorate and a solvent;
b) heating the mixture and maintaining at the same temperature to obtain a reaction mass;
c) isolating the deuterated ammonium perchlorate (ND₄ClO₄) from the reaction mass to obtain an isolated deuterated ammonium perchlorate (ND₄ClO₄); and
d) drying the isolated deuterated ammonium perchlorate (ND₄ClO₄) to obtain deuterated ammonium perchlorate (ND₄ClO₄) which having IP 95% to 98%.
2. The process as claimed in claim 1, wherein the making a mixture comprising ammonium perchlorate and a solvent is carried out at a temperature in the range of 10oC to 25oC.
3. The process as claimed in claim 1, wherein heating the mixture and maintaining the same temperature to obtain a reaction mass is carried out at a temperature in the range of 20oC to 35oC for a time period in the range of 10 hrs to 14 hrs.
4. The process as claimed in claim 1, wherein isolating the deuterated ammonium perchlorate (ND₄ClO₄) from the reaction mass to obtain isolated deuterated ammonium perchlorate (ND₄ClO₄) is carried out by distilling the solvent under vacuum at a temperature in the range of 20oC to 35oC.
5. The process as claimed in claim 1, wherein drying the isolated deuterated ammonium perchlorate (ND₄ClO₄) to obtain deuterated ammonium perchlorate (ND₄ClO₄) which having IP 95-98% is carried out under vacuum.
6. The process as claimed in claim 1, wherein solvent is selected from water, alcohols, ethers, ketones, acids, esters, acetonitrile (ACN), halogenated solvent(s) and/or deuterated form of water, alcohols, ethers, ketones, acids, esters, and/or deuterated halogenated solvent(s).
7. The process as claimed in claim 5, wherein the solvent is deuterated water (D2O).