CN102827038B - Preparation process for nitroguanidine - Google Patents
Preparation process for nitroguanidine Download PDFInfo
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- CN102827038B CN102827038B CN201210311021.6A CN201210311021A CN102827038B CN 102827038 B CN102827038 B CN 102827038B CN 201210311021 A CN201210311021 A CN 201210311021A CN 102827038 B CN102827038 B CN 102827038B
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- nitroguanidine
- washing
- nitric acid
- temperature
- mass concentration
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- IDCPFAYURAQKDZ-UHFFFAOYSA-N 1-nitroguanidine Chemical compound NC(=N)N[N+]([O-])=O IDCPFAYURAQKDZ-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 39
- 239000013078 crystal Substances 0.000 claims abstract description 29
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 27
- 238000005406 washing Methods 0.000 claims abstract description 27
- 238000002425 crystallisation Methods 0.000 claims abstract description 21
- 230000008025 crystallization Effects 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000009835 boiling Methods 0.000 claims description 35
- 238000001914 filtration Methods 0.000 claims description 24
- 238000000926 separation method Methods 0.000 claims description 19
- 239000008399 tap water Substances 0.000 claims description 12
- 235000020679 tap water Nutrition 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000011521 glass Substances 0.000 claims description 10
- MJFQUUWPZOGYQT-UHFFFAOYSA-O diaminomethylideneazanium;nitrate Chemical compound NC(N)=[NH2+].[O-][N+]([O-])=O MJFQUUWPZOGYQT-UHFFFAOYSA-O 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000007858 starting material Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 230000000384 rearing effect Effects 0.000 claims description 2
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002360 explosive Substances 0.000 abstract description 3
- 239000012295 chemical reaction liquid Substances 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 24
- 238000004519 manufacturing process Methods 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 6
- 229910002651 NO3 Inorganic materials 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation process for a single-compound explosive, i.e., nitroguanidine. In the process, the nitroguanidine is prepared by adopting a nitric acid method. A technical process comprises the following steps of: synthesizing nitroguanidine; controlling the crystallization of the nitroguanidine; washing the nitroguanidine; and drying the nitroguanidine. The process mainly comprises the following steps of: controlling process parameters such as temperature, stirring speed, dripping speed and the like in a crystallizing process; preparing a dilute nitric acid base solution of a proper mass concentration; and dripping a nitroguanidine reaction liquid into the nitric acid base solution for crystallizing, washing and drying to directly obtain a beta crystal form nitroguanidine product of which the purity is higher than 99 percent, the acidity is less than 0.06 percent and the granularity is 4-6 mum and which meets the requirements of a national military standard. Due to the adoption of the preparation process, energy consumption and secondary pollution caused by secondary crystallization due to unqualified granularity, acidity and purity of the crude nitroguanidine in the conventional process are avoided.
Description
Technical field
The invention belongs to fiery explosive technical field, relate to a kind of technique that adopts nitrate method to prepare nitroguanidine, the nitroguanidine that adopts this technique to prepare, primary crystallization can make the qualified product of beta crystal.
Background technology
Nitroguanidine is a kind of energetic material that is widely used in propelling charge, propelling agent and explosive.Meanwhile, also as gas generating agent component, be widely applied in the gas-bag system of Motor vehicles or aircraft.The derivative of nitroguanidine is also applied to industry-by-industry, as aspects such as medicine, agricultural chemicals.
Domestic nitroguanidine manufacturing enterprise, utilize sulfuric acid process to prepare nitroguanidine, in production process, to produce a large amount of Waste Sulfuric Acids (it is 16% dilute sulphuric acid and 10 tons of waste water containing nitroguanidine that 1 ton of nitroguanidine of every production produces approximately 23 tons of mass concentrations), serious to equipment corrosion, the mass concentration producing is that 16% Waste Sulfuric Acid is difficult for concentration and recovery recycling, need to use in lime and rear discharge, cause environmental pollution and the wasting of resources.And the alpha-crystal form nitroguanidine that sulfuric acid process obtains does not meet national military standard service requirements, need to crude product nitroguanidine, carry out secondary crystal with polyvinyl alcohol water solution, in secondary crystal, need to adopt mist projection granulating, just can obtain qualified nitroguanidine.In secondary crystal process, produce a large amount of containing nitroguanidine waste water, to environment structure severe contamination; In secondary crystal process, increase operation steps, used polyvinyl alcohol water solution, brought production cost significantly to increase; In secondary crystal process, be dissolved in polyvinyl alcohol water solution cannot crystallization for part nitroguanidine, and crystallization yield is reduced; Increased danger simultaneously.
Chinese patent application (publication number: disclose a kind of friendly process of producing nitroguanidine CN101497549A), the method utilizes nitrate method to prepare nitroguanidine, but there is no crystallization control process, gained nitroguanidine crude product can not meet military standard of China, need carry out secondary crystal and refine.In secondary crystal, need to adopt polyvinyl alcohol water solution secondary crystal just can obtain qualified nitroguanidine.In secondary crystal process, produce a large amount of containing nitroguanidine waste water, to environment structure severe contamination; In secondary crystal process, use polyvinyl alcohol water solution, brought production cost significantly to increase; In secondary crystal process, be dissolved in polyvinyl alcohol water solution cannot crystallization for part nitroguanidine, and crystallization yield is reduced; Increased danger simultaneously.
Summary of the invention
For existing defect or the deficiency of preparing the existence of nitroguanidine method, the object of the invention is to, provide a kind of simple employing nitrate method to prepare the technique of nitroguanidine, by to effectively the controlling of nitroguanidine crystallisation process, washing process condition, primary crystallization obtains qualified beta crystal nitroguanidine product.Solved in current technology route length, secondary crystal process and produced the problems such as a large amount of waste water and pollution.Shorten operational path, reduced production cost, guaranteed quality product.
In order to realize above-mentioned task, the present invention takes following technical solution:
A preparation technology, is characterized in that, specifically follows these steps to carry out:
1) prepare the starting material of nitroguanidine: the concentrated nitric acid that mass concentration is 60% ~ 98%; Powdery Guanidinium nitrate; Mass concentration is rare nitric acid of 30%; Mass concentration is 2% ~ 5% Na
2cO
3solution;
2) nitroguanidine building-up process is: first connect low temperature bath power supply, temperature is adjusted to below 10 ℃, the concentrated nitric acid that is 60% ~ 98% by 90ml mass concentration joins in 250ml four-hole boiling flask, start number and write agitator, stirring rake material is tetrafluoroethylene, adjusting rotary speed is to 270rpm ~ 350rpm, add Guanidinium nitrate 30g, control feed rate and be less than or equal to 15 ℃ with temperature, after reinforced, low temperature bath temperature is adjusted to 45 ℃, when being warming up to 43 ℃, reaction solution starts reaction, reaction times is 30min, by low temperature bath, nitroguanidine reaction solution is cooled to-3 ℃~-7 ℃.
3) nitroguanidine crystallization control process is: the concentration that the reaction solution of nitroguanidine is dropped to 360ml ~ 450ml is in 20%~40% rare nitric acid, crystallization control system temperature is at-3 ℃~-7 ℃, control rate of addition at 0.5ml/min ~ 5ml/min, stirring velocity is controlled, and rotating speed maintains 600rpm ~ 800rpm left and right.In dropping process, can produce nitroguanidine white crystal.
4) after the reaction solution of nitroguanidine is added dropwise to complete, continue to stir with 600rpm ~ 800rpm speed, temperature is at-3 ℃~-7 ℃, and this process is called growing the grain, and rearing crystal time is 120min ~ 240min.Through the growing the grain of 120min ~ 240min, filtering separation spent acid wherein, can obtain containing aci nitro guanidine.
5) nitroguanidine washing process is: filtering separation is obtained containing aci nitro guanidine, add in 250ml four-hole boiling flask, with the tap water machinery agitator treating under normal temperature, by water-in, add water 135ml, churning time is 15min, and mixing speed is controlled at 900rpm ~ 1200rpm, filtering separation after washing, filtration product is joined in 250ml four-hole boiling flask again to washing again in the same way, its tap water machinery agitator treating totally 3 times.
The 4th is with same mode of washing, and in tap water, adding mass concentration is 2% ~ 5% Na
2cO
3solution is washed 1 time, after washing, carries out filtering separation, obtains wet product nitroguanidine.
6) nitroguanidine drying process is: the wet product nitroguanidine that washing is obtained, putting into watch-glass weighs with electronic scales, oven temperature is risen to 60 ℃, the watch-glass that fills wet product nitroguanidine is placed in baking oven, 6h, can obtain purity and be greater than 99% time of drying, and acidity is less than 0.06%, granularity, at 4 μ m ~ 6 μ m, meets the beta crystal nitroguanidine product of military standard of China.
Nitroguanidine crystallization control technique of the present invention, operational path is short, primary crystallization, has reduced production process, directly obtains qualified beta crystal nitroguanidine product, because processing step is few, improve yield, effectively reduced the wastewater discharge in nitroguanidine preparation process, reduced environmental pollution, save production cost, eliminated the danger in secondary crystal process.
Embodiment
Below in conjunction with embodiment, the present invention is done further to discuss in detail.
In following embodiment, the starting material of preparing nitroguanidine are: the concentrated nitric acid that mass concentration is 60% ~ 98%; Powdery Guanidinium nitrate; Mass concentration is rare nitric acid of 30%; Na
2cO
3solution;
Starting material are prepared: with graduated cylinder, measure respectively the concentrated nitric acid that the mass concentration of 90ml is 60% ~ 98% stand-by, take Guanidinium nitrate 30g stand-by, the Na that rare nitric acid that preparation mass concentration is 30% and mass concentration are 2% ~ 5% with electronic scales
2cO
3solution for later use.
Main laboratory apparatus of the present invention: 250ml four-hole boiling flask, 1L four-hole boiling flask low temperature bath, number are write agitator, thermometer, graduated cylinder, electronic scales, suction filter pump, water-bath baking oven.
Below the embodiment that contriver provides.It should be noted that, the invention is not restricted to these embodiment, certainly, according to technical scheme of the present invention, can also amplify production.
Embodiment 1:
The present embodiment carries out as follows:
(1) 250ml four-hole boiling flask is placed in to low temperature bath, temperature is adjusted to below 10 ℃.
(2) by load weighted 90ml mass concentration, be 98%HNO
3, join in four-hole boiling flask.
(3) when 250ml four-hole boiling flask nitric acid temperature is down in 10 ℃, by load weighted 30g Guanidinium nitrate, slowly add in four-hole boiling flask, mixing speed is adjusted to 350rpm, and reacting liquid temperature is controlled at below 15 ℃.
(4) after reinforced, low temperature bath is warming up to 45 ℃.When reaction solution is warming up to 43 ℃ in four-hole boiling flask, start reaction, the reaction times amounts to 30min.
(5) after completion of the reaction, low temperature bath is adjusted to-3 ℃, reacting liquid temperature is down to-3 ℃.
(6) 1L four-hole boiling flask is put into low temperature bath, the rare nitric acid that is 20% by 360ml mass concentration adds in 1L four-hole boiling flask, and mixing speed is 600rpm.
(7) when rare nitric acid temperature is down to-3 ± 1 ℃, nitroguanidine reaction solution is dripped in rare nitric acid.Rate of addition is 0.5ml ~ 2ml/min, keeps crystallizing system temperature in-3 ± 1 ℃.Drip after certain hour, start to occur nitroguanidine crystallization, continue to drip nitroguanidine reaction solution, until nitroguanidine reaction solution dropwises.
(8) after nitroguanidine reaction solution dropwises, continue to keep stirring velocity and temperature, start growing the grain, growing the grain 120min.
(9), after growing the grain finishes, filtering separation obtains containing aci nitro guanidine.
(10) filtering separation is obtained containing aci nitro guanidine, add in 250ml four-hole boiling flask, with the tap water machinery agitator treating under normal temperature, by water-in, add water 135ml, churning time is 15min, and mixing speed is controlled at 1200rpm, filtering separation after washing, filtration product is joined in 250ml four-hole boiling flask again, wash altogether in the same way 3 times.
The 4th is with same mode of washing, and in tap water, adding mass concentration is 5% Na
2cO
3solution is washed 1 time, after washing, carries out filtering separation, obtains wet product nitroguanidine.
(11) wet product nitroguanidine washing being obtained is put into watch-glass and is weighed with electronic scales, and oven temperature is risen to 60 ℃, the watch-glass that fills wet product nitroguanidine is placed in baking oven, time of drying 6h.Obtain purity and be greater than 99%, acidity is less than 0.06%, and granularity is at 4 μ m ~ 6 μ m, and meets the beta crystal nitroguanidine product of military standard of China.
Embodiment 2:
The present embodiment carries out as follows:
(1) 250ml four-hole boiling flask is placed in to low temperature bath, temperature is adjusted to below 10 ℃.
(2) by load weighted 90ml mass concentration, be 80%HNO
3, join in four-hole boiling flask.
(3) when 250ml four-hole boiling flask nitric acid temperature is down to below 10 ℃, by load weighted 30g Guanidinium nitrate, slowly add in four-hole boiling flask, mixing speed is adjusted to 300rpm, and reacting liquid temperature is controlled at below 15 ℃.
(4) after reinforced, low temperature bath is warming up to 45 ℃.When reaction solution is warming up to 43 ℃ in four-hole boiling flask, start reaction.Reaction times amounts to 30min.
(5) after completion of the reaction,, by-5 ± 1 ℃ of low temperature bath modulation, reacting liquid temperature is down to-5 ± 1 ℃.
(6) 1L four-hole boiling flask is put into low temperature bath, the rare nitric acid that is 30% by 400ml mass concentration adds in 1L four-hole boiling flask, and mixing speed is 700rpm.
(7) when rare nitric acid temperature is down to-5 ± 1 ℃, nitroguanidine reaction solution is dripped in rare nitric acid.Rate of addition is 2ml ~ 3.5ml/min, keeps crystallizing system temperature in-5 ± 1 ℃.Drip after certain hour, start to occur nitroguanidine crystallization, continue to drip nitroguanidine reaction solution, until nitroguanidine reaction solution dropwises.
(8) after nitroguanidine reaction solution dropwises, continue to keep stirring velocity and temperature, start growing the grain, growing the grain 180min.
(9), after growing the grain finishes, filtering separation obtains containing aci nitro guanidine.
(10) filtering separation is obtained containing aci nitro guanidine, add in 250ml four-hole boiling flask, with the tap water machinery agitator treating under normal temperature, by water-in, add water 135ml, churning time is 15min, and mixing speed is controlled at 1000rpm, filtering separation after washing, filtration product is joined in 250ml four-hole boiling flask again, wash altogether in the same way 3 times.
The 4th is with same mode of washing, and in tap water, adding mass concentration is 3.5% Na
2cO
3solution is washed 1 time, after washing, carries out filtering separation, obtains wet product nitroguanidine.
(11) wet product nitroguanidine washing being obtained is put into watch-glass and is weighed with electronic scales, and oven temperature is risen to 60 ℃, the watch-glass that fills wet product nitroguanidine is placed in baking oven, time of drying 6h.Obtain purity and be greater than 99%, acidity is less than 0.06%, and granularity is at 4 μ m ~ 6 μ m, and meets the beta crystal nitroguanidine product of military standard of China.Embodiment 3:
The present embodiment carries out as follows:
(1) 250ml four-hole boiling flask is placed in to low temperature bath, temperature is adjusted to below 10 ℃.
(2) by load weighted 90ml mass concentration, be 60%HNO
3, join in four-hole boiling flask.
(3) when 250ml four-hole boiling flask nitric acid temperature is down in 10 ℃, by load weighted 30g Guanidinium nitrate, slowly add in four-hole boiling flask, mixing speed is adjusted to 270rpm, and reacting liquid temperature is controlled at below 15 ℃.
(4) after reinforced, low temperature bath is warming up to 45 ℃.When reaction solution is warming up to 43 ℃ in four-hole boiling flask, start reaction, the reaction times amounts to 30min.
(5) after completion of the reaction,, by-7 ± 1 ℃ of low temperature bath modulation, reacting liquid temperature is down to-7 ± 1 ℃.
(6) 1L four-hole boiling flask is put into low temperature bath, the rare nitric acid that is 40% by 450ml mass concentration adds in 1L four-hole boiling flask, and mixing speed is 800rpm.
(7) when rare nitric acid temperature is down to-7 ± 1 ℃, nitroguanidine reaction solution is dripped in rare nitric acid.Rate of addition is 3.5ml ~ 5ml/min, keeps crystallizing system temperature in-7 ± 1 ℃.Drip after certain hour, start to occur nitroguanidine crystallization, continue to drip nitroguanidine reaction solution, until nitroguanidine reaction solution dropwises.
(8) after nitroguanidine reaction solution dropwises, continue to keep stirring velocity and temperature, start growing the grain, growing the grain 240min.
(9), after growing the grain finishes, filtering separation obtains containing aci nitro guanidine.
(10) filtering separation is obtained containing aci nitro guanidine, add in 250ml four-hole boiling flask, with the tap water machinery agitator treating under normal temperature, by water-in, add water 135ml, churning time is 15min, and mixing speed is controlled at 900rpm, filtering separation after washing, filtration product is joined in 250ml four-hole boiling flask again, wash in the same way 3 times.
The 4th is with same mode of washing, and in tap water, adding mass concentration is 2% Na
2cO
3solution is washed 1 time, after washing, carries out filtering separation, obtains wet product nitroguanidine.
(11) wet product nitroguanidine washing being obtained is put into watch-glass and is weighed with electronic scales, and oven temperature is risen to 60 ℃, the watch-glass that fills wet product nitroguanidine is placed in baking oven, time of drying 6h.Can obtain purity and be greater than 99%, acidity is less than 0.06%, and granularity, at 4 μ m ~ 6 μ m, meets the beta crystal nitroguanidine product that national military standard is used.
The nitroguanidine crystallization control technique that above-described embodiment provides, operational path is short, reduced production process, primary crystallization directly obtains qualified beta crystal nitroguanidine, effectively reduce the quantity discharged containing nitroguanidine waste water, reduce environmental pollution, saved production cost, eliminated the danger in secondary crystal process.
Claims (1)
1. a nitroguanidine preparation technology, is characterized in that, specifically follows these steps to carry out:
1) prepare the starting material of nitroguanidine: the concentrated nitric acid that mass concentration is 60% ~ 98%; Powdery Guanidinium nitrate; Mass concentration is rare nitric acid of 20% ~ 40%; Mass concentration is 2% ~ 5% Na
2cO
3solution;
2) nitroguanidine building-up process is: low temperature bath temperature is adjusted to below 10 ℃, the concentrated nitric acid of 90ml is joined in 250ml four-hole boiling flask, start agitator, stirring rake material is tetrafluoroethylene, adjusting rotary speed is to 270rpm ~ 350rpm, add Guanidinium nitrate 30g, control feed rate and be no more than 15 ℃ with temperature, after reinforced, low temperature bath temperature is adjusted to 45 ℃, when being warming up to 43 ℃, reaction solution starts reaction, reaction times is 30min, after having reacted, by low temperature bath, nitroguanidine reaction solution is cooled to-3 ℃~-7 ℃;
3) nitroguanidine crystallization control process is: the reaction solution of nitroguanidine is dropped in rare nitric acid of 360ml ~ 450ml, crystallization control system temperature is at-3 ℃~-7 ℃, control rate of addition at 0.5ml/min ~ 5ml/min, and stirring velocity is maintained to 600rpm ~ 800rpm, in the reaction solution dropping process of nitroguanidine, produce nitroguanidine white crystal;
4) after the reaction solution of nitroguanidine is added dropwise to complete, continue to stir with 600rpm ~ 800rpm speed, temperature is controlled at-3 ℃~-7 ℃, and this process is called growing the grain, and rearing crystal time is 120min ~ 240min; After growing the grain completes, filtering separation spent acid, obtains containing aci nitro guanidine;
5) nitroguanidine washing process is: by obtain containing aci nitro guanidine, add in 250ml four-hole boiling flask, under normal temperature, use tap water machinery agitator treating, by water-in, add water 135ml, churning time is 15min, and mixing speed is controlled at 900rpm ~ 1200rpm, filtering separation after washing, filtration product is joined in 250ml four-hole boiling flask again to washing again in the same way, its tap water machinery agitator treating totally 3 times;
The 4th is with same mode of washing, and in tap water, adding mass concentration is 2% ~ 5% Na
2cO
3solution is washed 1 time, after washing, carries out filtering separation, obtains wet product nitroguanidine;
6) nitroguanidine drying process is: by the wet product nitroguanidine after washing, putting into watch-glass weighs with electronic scales, oven temperature is risen to 60 ℃, the watch-glass that fills wet product nitroguanidine is placed in baking oven, 6h, obtained purity and was greater than 99% time of drying, and acidity is less than 0.06%, granularity is at 4 μ m ~ 6 μ m, and meets the beta crystal nitroguanidine product of military standard of China.
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CN103696014B (en) * | 2013-12-12 | 2015-12-30 | 宁夏贝利特化工有限公司 | By the method for producing nitroguanidine, the waste of Dyhard RU 100 produces calcium sulfate crystal whiskers and calcium sulfate |
CN103787922B (en) * | 2014-03-04 | 2016-06-01 | 新昌县鸿吉电子科技有限公司 | A kind of Industrial Catalysis method of synthesizing nitryl substitution compound |
CN104860849A (en) * | 2015-06-04 | 2015-08-26 | 西安近代化学研究所 | Continuous crystallization process for preparing nitroguanidine through nitric acid method |
CN107721884B (en) * | 2017-11-06 | 2020-05-05 | 西安近代化学研究所 | Nitroguanidine engineering production process |
CN112851554A (en) * | 2019-11-28 | 2021-05-28 | 昆山昆化有限公司 | Preparation method of guanidine nitrate |
CN112920091A (en) * | 2020-12-31 | 2021-06-08 | 宁夏天泽新材料科技有限公司 | Preparation process of nitroguanidine |
CN112778165A (en) * | 2021-01-11 | 2021-05-11 | 宁夏贝利特生物科技有限公司 | Preparation method of superfine nitroguanidine |
CN115819287A (en) * | 2022-11-28 | 2023-03-21 | 贝利特化学股份有限公司 | Superfine columnar nitroguanidine and preparation method thereof |
CN115724773A (en) * | 2022-12-05 | 2023-03-03 | 宁夏东吴农化股份有限公司 | Method for preparing superfine nitroguanidine by virtue of supergravity hydrolytic crystallization method |
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WO2001046129A2 (en) * | 1999-12-20 | 2001-06-28 | Dynamit Nobel Gmbh Explosivstoff- Und Systemtechnik | Method for producing nitroguanidine |
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GB2006201A (en) * | 1977-10-12 | 1979-05-02 | Nigu Chemie Gmbh | Production of nitroguanidine from guanidine nitrate and nitric acid |
CN87103545A (en) * | 1987-05-18 | 1988-11-30 | 西安近代化学研究所 | Continuous process for preparing nitroguanidine in pipeline |
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