CN115925644B - Method for preparing flame retardant by using amine waste mother liquor - Google Patents
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- CN115925644B CN115925644B CN202211455622.4A CN202211455622A CN115925644B CN 115925644 B CN115925644 B CN 115925644B CN 202211455622 A CN202211455622 A CN 202211455622A CN 115925644 B CN115925644 B CN 115925644B
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- 239000002699 waste material Substances 0.000 title claims abstract description 41
- 239000003063 flame retardant Substances 0.000 title claims abstract description 40
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- 238000000034 method Methods 0.000 title claims abstract description 37
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- 150000001412 amines Chemical class 0.000 title claims abstract description 23
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- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 39
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 claims abstract description 37
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims abstract description 25
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 28
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- 239000000047 product Substances 0.000 claims description 22
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- 238000006116 polymerization reaction Methods 0.000 claims description 18
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 238000003828 vacuum filtration Methods 0.000 claims description 4
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 3
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
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- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
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- NDEMNVPZDAFUKN-UHFFFAOYSA-N guanidine;nitric acid Chemical compound NC(N)=N.O[N+]([O-])=O.O[N+]([O-])=O NDEMNVPZDAFUKN-UHFFFAOYSA-N 0.000 description 1
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- Fertilizers (AREA)
Abstract
The invention discloses a method for preparing a flame retardant by utilizing amine waste mother liquor, which belongs to the technical field of melamine cyanurate flame retardants, and comprises the following steps: generating cyanamide, generating melamine and generating a flame retardant; the invention can realize the full effective recovery and utilization of products and materials in the waste mother liquor, reduce the discharge of waste water, and the recovered flame retardant melamine cyanurate has high yield, good quality, mild reaction conditions and easy operation of equipment, and the obtained products can be used for industrialized application.
Description
Technical Field
The invention relates to the technical field of melamine cyanurate flame retardants, in particular to a method for preparing a flame retardant by using amine waste mother liquor.
Background
Dicyandiamide cyanoguanidine, also known as dicyandiamide, has a molecular formula of C 2H4N4. Dicyandiamide is white crystal with melting point of 207-209 deg.c, and is stable in dry product and soluble in water and ethanol when heated.
The main uses of dicyandiamide are:
(1) Can be used as flocculant for water treatment;
(2) The method is used as a dye fixing agent and a latent curing agent of an epoxy resin adhesive to prepare a single-component epoxy adhesive;
(3) The fertilizer can control the activity of nitrifying bacteria, so that the conversion speed of nitrogen fertilizer in soil is regulated, the loss of nitrogen is reduced, and the use efficiency of the fertilizer is improved;
(4) As fine chemical intermediate, the said product may be used in preparing guanidine nitrate, sulfonamides, thiourea, nitrocellulose stabilizer, rubber vulcanization accelerator, steel surface hardening agent, artificial leather stuffing, adhesive, etc.
Melamine Cyanurate (MCA) is a typical halogen-free, environmentally friendly nitrogen-based flame retardant, which is a white uniform particle or a white flowing powder with a greasy feel. Is insoluble in water, but soluble in organic solvents such as ethanol and formaldehyde. MCA was originally used as a solid lubricant, and later gradually applied to materials such as rubber, polyamide, epoxy resin, polyamide, etc. as a flame retardant component. Because of its high nitrogen content, good flame retardant effect, environmental friendliness, low price, etc., it is often used to flame retardant polyamide 6 (PA 6) and polyamide 66 (PA 66). The MCA structural formula and hydrogen bond cross-linked network are shown below:
currently, the traditional process for preparing dicyandiamide is a batch operation mode, the starting material is lime nitrogen (active ingredient calcium cyanamide), and the operation steps can be divided into a three-step method and a four-step method. The three-step method is divided into three stages of hydrolysis decalcification, polymerization and crystallization; the four-step method is divided into four stages of hydrolysis, decalcification, polymerization and crystallization, namely the four-step method separates the two processes of hydrolysis and decalcification.
However, in any method, all steps related to the production of the product adopt water as a solvent, a large amount of mother liquor is generated in the cooling crystallization separation stage, and the mother liquor contains a large amount of impurities including 5.5-8.5% (w/w) of urea, 0.5-1.0% (w/w) of melamine, 0.6-1.2% (w/w) of mono-cyanamide, and 4.5-5.0% (w/w) of dicyandiamide and other small amount of impurities after being reused for many times. The high impurity content in the mother solution can cause precipitation of impurities along with dicyandiamide in the product during crystallization, so that the standard exceeding of various impurities in dicyandiamide is caused, and the quality index of dicyandiamide is seriously influenced.
If the waste mother liquor is directly used for sewage treatment, resources are wasted, the sewage treatment cost of enterprises can be increased, and the environmental pollution load is increased. With the development of dicyandiamide industry and the expansion of production scale, the yield of waste mother liquor is gradually improved. How to treat dicyandiamide waste mother liquor effectively is a great difficulty of whether enterprises can develop health and durability.
Therefore, it is necessary to provide a new treatment mode of the amine waste mother liquor, so that the defect caused by treatment of the amine waste mother liquor in a sewage treatment plant can be overcome, impurities in the amine waste mother liquor are comprehensively recovered and converted into other useful substances, certain economic benefits are created, sewage treatment cost is reduced, and the influence on the environment is reduced, thereby achieving the beneficial effects of improving the product quality and the product competitiveness.
Through searching, no technology is disclosed at present for recycling waste mother liquor generated in the amine production process.
The prior art describes the preparation of melamine cyanurate as follows:
Chinese patent CN109438379a discloses a process for preparing melamine cyanurate: (a) Adding melamine and cyanuric acid into a container, stirring and grinding uniformly; (b) adding a chain extender into the container, and uniformly stirring; (c) Adding deionized water into the container, and regulating the pH value to be neutral; (d) Stirring uniformly, sealing, and standing for 3-10 days at room temperature; (e) And after the reaction is finished, drying and grinding to obtain a melamine cyanurate finished product.
Chinese patent CN106749061a discloses a method for synthesizing melamine cyanurate fire retardant by solid phase synthesis, i.e. under anhydrous condition, using specific mechanical equipment to synthesize melamine cyanurate from melamine and cyanuric acid.
In the above disclosed technology, melamine cyanurate can be obtained, but the above technology has problems of using a chain extender, having a long reaction time (3 to 10 days), having high equipment purchase cost, having low equipment utilization rate, having large energy consumption, and the like, and is not used for industrial production.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for preparing a flame retardant by using an amine waste mother solution, which can realize the full effective recovery and utilization of products and materials in the waste mother solution, reduce the emission of waste water, and has the advantages of high yield, good quality, mild reaction conditions and easy operation of equipment of the recovered flame retardant melamine cyanurate, and the obtained product can be used for industrial application.
In order to solve the technical problems, the invention adopts the following technical scheme:
A method for preparing a flame retardant by utilizing amine waste mother liquor comprises the following steps: the formation of cyanamide, melamine and flame retardant.
Adding an acidic substance into the waste mother liquor to adjust the pH to 7.0-8.0, stirring for 10min, vacuum-filtering to obtain filtrate, performing low-temperature negative pressure distillation on the filtrate, controlling the temperature in the low-temperature negative pressure distillation to be 40-45 ℃, controlling the negative pressure to be minus 0.085-minus 0.10MPa, and ending the low-temperature negative pressure distillation to obtain a concentrated solution A; adding lime nitrogen into drinking water, maintaining the temperature at 30-40 ℃ and stirring for 30-60 min, introducing carbon dioxide at a speed of 5mL/min to adjust PH=7.0-8.0, and carrying out vacuum suction filtration to obtain filtrate B;
in the process of generating the cyanamide, the waste mother liquor comprises the following components in percentage by mass: 1.2% of dicyandiamide, 4.6% of dicyandiamide, 0.8% of melamine, 7.1% of urea and 0.1% of other impurities;
In the process of generating the cyanamide, the content of calcium cyanamide in the lime nitrogen is 61%;
in the generated cyanamide, the cyanamide content in the filtrate B is 3.1-3.4%;
In the process of generating the cyanamide, the acidic substance is one of carbon dioxide or sulfuric acid, and when the acidic substance is carbon dioxide, the carbon dioxide is introduced at a speed of 5mL/min;
in the process of generating the cyanamide, the weight ratio of the waste mother solution to the concentrated solution A is 600:300;
In the produced cyanamide, the weight ratio of the drinking water to the lime nitrogen is 200:20.
Sequentially adding the concentrated solution A and the filtrate B into a high-pressure container, adding drinking water and a catalyst for high-pressure polymerization, controlling the temperature of the high-pressure polymerization to be 125-135 ℃, controlling the pressure to be 0.25-0.36 Mpa, and controlling the time to be 2-3 h, thus obtaining feed liquid of the melamine after the high-pressure polymerization is finished;
in the melamine production, the melamine content in the melamine feed liquid is 6.4-6.6%;
The weight ratio of the concentrated solution A in the melamine production to the lime nitrogen in the cyanamide production is 300:20;
in the melamine production, the mass volume ratio of the concentrated solution A to the drinking water to the catalyst is 300g:200 mL:0.1-0.2 g;
In the melamine production, the catalyst is one of aluminum oxide or aluminum silicate.
Continuously heating the melamine feed liquid to 160-170 ℃ in a high-pressure container, controlling the pressure in the high-pressure container to 0.60-0.71 Mpa, preserving heat for 2.5-3.5 h to obtain melamine cyanurate feed liquid, cooling to 10-20 ℃, preserving heat for 0.5-1.5 h at 10-20 ℃, and performing suction filtration, hot water washing and drying to obtain melamine cyanurate products;
in the flame retardant, the content of melamine cyanurate in the melamine cyanurate product is 99.0-99.5%.
A method for preparing a flame retardant by utilizing amine waste mother liquor comprises the following reaction routes:
The calcium cyanamide is hydrolyzed and decalcified to generate cyanamide:
2CaCN2+ 2H2O = Ca(HCN2)2+ Ca(OH)2
Ca(HCN2)2+ CO2+ H2O = H2CN2+ CaCO3↓
polymerization of dicyandiamide with dicyandiamide to form melamine:
urea is pyrolyzed to generate cyanuric acid, and cyanuric acid and melamine hydrogen bond are subjected to a compound reaction to generate melamine cyanurate:
compared with the prior art, the invention has the following beneficial effects:
(1) According to the method for preparing the flame retardant by utilizing the amine waste mother liquor, provided by the invention, a proper amount of lime nitrogen is added for directional reaction, and distilled water and final filtrate obtained in the treatment process are used for recycling dicyandiamide products, so that all the products and materials in the waste mother liquor are effectively recycled and utilized, and the waste water emission is reduced;
(2) According to the method for preparing the flame retardant by utilizing the amine waste mother liquor, the melamine is subjected to hydrogen bond recombination reaction to generate the melamine cyanurate product, and the content of melamine cyanurate in the obtained melamine cyanurate product can reach 99.0-99.5%, so that the method can be continuously used for industrialization;
(3) According to the method for preparing the flame retardant by utilizing the amine waste mother liquor, the yield of the finally obtained melamine cyanurate flame retardant is high and can reach 81.1-85.0%.
Detailed Description
Example 1
A method for preparing a flame retardant by utilizing amine waste mother liquor specifically comprises the following steps:
1. Production of cyanamide
600G of waste mother liquor is added into a dry three-mouth bottle, carbon dioxide is introduced at the speed of 5mL/min to adjust the PH=7.0, then the mixture is stirred for 10min and then is subjected to vacuum filtration, and the filtrate is subjected to low-temperature negative pressure distillation under the conditions that the temperature is 40 ℃ and the negative pressure is minus 0.085 to minus 0.090MPa, so that a concentrated solution A with the weight of 300g is obtained;
the waste mother solution comprises the following components in percentage by mass: 1.2% of dicyandiamide, 4.6% of dicyandiamide, 0.8% of melamine, 7.1% of urea and 0.1% of other impurities (mainly amine compounds);
Adding 20g of lime nitrogen into 200g of drinking water, keeping the temperature at 30 ℃ and stirring for 30min, introducing carbon dioxide at a speed of 5mL/min to adjust the PH to be 7.0, and carrying out vacuum suction filtration to obtain filtrate B with the cyanamide content of 3.2%;
the content of calcium cyanamide in the lime nitrogen is 61%.
2. Melamine formation
And (3) sequentially adding the concentrated solution A and the filtrate B obtained in the step 1 into an autoclave, adding 200ml of drinking water and 0.1g of aluminum oxide catalyst, then performing high-pressure polymerization, controlling the temperature of the high-pressure polymerization to be 125 ℃, controlling the pressure to be 0.25Mpa, and controlling the time to be 2 hours, wherein the high-pressure polymerization is finished to obtain the feed liquid of melamine with the content of 6.5%.
3. To produce the flame retardant
Continuously heating the feed liquid of the melamine in the step 2 to 160 ℃ in an autoclave, controlling the pressure in the autoclave to be 0.60Mpa, preserving heat for 2.5h to obtain the feed liquid converted into melamine cyanurate, cooling to 10 ℃, preserving heat for 0.5h at 10 ℃, and then carrying out suction filtration, hot water washing and drying to obtain 68.7g of melamine cyanurate product, wherein the yield is 82.1% (calculated by dicyandiamide), and the content of melamine cyanurate in the melamine cyanurate product is 99.2 percent according to HG/T5341-2018 detection.
Example 2
A method for preparing a flame retardant by utilizing amine waste mother liquor specifically comprises the following steps:
1. Production of cyanamide
600G of waste mother liquor is added into a dry three-mouth bottle, carbon dioxide is introduced at the speed of 5mL/min to adjust the PH=7.5, then the mixture is stirred for 10min and then is subjected to vacuum filtration, and the filtrate is subjected to low-temperature negative pressure distillation under the conditions that the temperature is 42 ℃ and the negative pressure is minus 0.090 to minus 0.095MPa, so that a concentrated solution A with the weight of 300g is obtained;
the waste mother solution comprises the following components in percentage by mass: 1.2% of dicyandiamide, 4.6% of dicyandiamide, 0.8% of melamine, 7.1% of urea and 0.1% of other impurities (mainly amine compounds);
adding 20g of lime nitrogen into 200g of drinking water, keeping the temperature at 35 ℃ and stirring for 45min, introducing carbon dioxide at a speed of 5mL/min to adjust the PH to be 7.5, and carrying out vacuum suction filtration to obtain filtrate B with the cyanamide content of 3.1%;
the content of calcium cyanamide in the lime nitrogen is 61%.
2. Melamine formation
And (3) sequentially adding the concentrated solution A and the filtrate B obtained in the step 1 into an autoclave, adding 200ml of drinking water and 0.2g of aluminum oxide catalyst, and then performing high-pressure polymerization, wherein the temperature of the high-pressure polymerization is controlled to be 130 ℃, the pressure is controlled to be 0.31Mpa, the time is 2.5h, and the high-pressure polymerization is finished to obtain the feed liquid of melamine with the content of 6.6%.
3. To produce the flame retardant
Continuously heating the feed liquid of the melamine in the step 2 to 165 ℃ in an autoclave, controlling the pressure in the autoclave to 0.66Mpa, preserving heat for 3.0h to obtain feed liquid converted into melamine cyanurate, cooling to 15 ℃, preserving heat for 1h at 15 ℃, and then carrying out suction filtration, hot water washing and drying to obtain 71.1g of melamine cyanurate product, wherein the yield is 85.0% (calculated by dicyandiamide), and the content of the melamine cyanurate in the melamine cyanurate product is 99.5 percent according to HG/T5341-2018 detection.
Example 3
A method for preparing a flame retardant by utilizing amine waste mother liquor specifically comprises the following steps:
1. Production of cyanamide
600G of waste mother liquor is added into a dry three-mouth bottle, the PH=8.0 is regulated by sulfuric acid, then the mixture is stirred for 10min and then is subjected to vacuum filtration, and filtrate is subjected to low-temperature negative pressure distillation under the conditions that the temperature is 45 ℃ and the negative pressure is-0.095 to-0.10 MPa, so that concentrated solution A with the weight of 300g is obtained;
the waste mother solution comprises the following components in percentage by mass: 1.2% of dicyandiamide, 4.6% of dicyandiamide, 0.8% of melamine, 7.1% of urea and 0.1% of other impurities (mainly amine compounds);
Adding 20g of lime nitrogen into 200g of drinking water, keeping the temperature at 40 ℃ and stirring for 60min, introducing carbon dioxide at a speed of 5mL/min to adjust the PH to be 8.0, and carrying out vacuum suction filtration to obtain filtrate B with the cyanamide content of 3.4%;
the content of calcium cyanamide in the lime nitrogen is 61%.
2. Melamine formation
Sequentially adding the concentrated solution A and the filtrate B obtained in the step 1 into an autoclave, adding 200ml of drinking water and 0.2g of aluminum silicate catalyst, and then performing high-pressure polymerization, wherein the temperature of the high-pressure polymerization is controlled to be 135 ℃, the pressure is controlled to be 0.36Mpa, the time is 3 hours, and the high-pressure polymerization is finished to obtain the feed liquid of melamine with the content of 6.4%.
3. To produce the flame retardant
Continuously heating the feed liquid of the melamine in the step 2 to 170 ℃ in an autoclave, controlling the pressure in the autoclave to 0.71Mpa, preserving heat for 3.5h to obtain feed liquid converted into melamine cyanurate, cooling to 20 ℃, preserving heat for 1.5h at 20 ℃, and then carrying out suction filtration, hot water washing and drying to obtain 67.9g of melamine cyanurate product, wherein the yield is 81.1% (calculated by dicyandiamide), and the content of the melamine cyanurate in the melamine cyanurate product is 99.0 percent according to HG/T5341-2018 detection.
From the results of the examples, it is understood that the temperature of the autoclave was raised to 130℃in the melamine-forming step of the 2 nd step of example 2, and the temperature of the autoclave was raised to 125℃in the melamine-forming step of the 2 nd step of example 1, and the total yield of example 2 was significantly higher than that of example 1, indicating that the preferable temperature in the melamine-forming step of the 2 nd step was 130 ℃.
The feed solution of melamine in the step 3 of producing flame retardant in example 3 was again heated to 170℃in the autoclave, and the feed solution of melamine in the step 3 of producing flame retardant in example 1 was again heated to 160℃in the autoclave, the overall yield of example 1 being significantly higher than that of example 3, indicating a preferred temperature of 170℃in the step 3 of producing flame retardant.
Claims (6)
1. The method for preparing the flame retardant by using the amine waste mother liquor is characterized by comprising the following steps of: generating cyanamide, generating melamine and generating a flame retardant;
Adding an acidic substance into the waste mother liquor to adjust the pH to 7.0-8.0, stirring for 10min, vacuum-filtering to obtain filtrate, performing low-temperature negative pressure distillation on the filtrate, controlling the temperature in the low-temperature negative pressure distillation to be 40-45 ℃, controlling the negative pressure to be minus 0.085-minus 0.10MPa, and ending the low-temperature negative pressure distillation to obtain a concentrated solution A; lime nitrogen is added into the drinking water, the temperature is maintained and the stirring is carried out, carbon dioxide is introduced to adjust the PH value to be 7.0-8.0, and the vacuum filtration is carried out, thus obtaining filtrate B;
the waste mother solution comprises the following components in percentage by mass: 1.2% of dicyandiamide, 4.6% of dicyandiamide, 0.8% of melamine, 7.1% of urea and 0.1% of other impurities;
Sequentially adding the concentrated solution A and the filtrate B into a high-pressure container, adding drinking water and a catalyst for high-pressure polymerization, controlling the temperature of the high-pressure polymerization to be 125-135 ℃, controlling the pressure to be 0.25-0.36 Mpa, and controlling the time to be 2-3 h, thus obtaining feed liquid of the melamine after the high-pressure polymerization is finished;
In the process of generating the cyanamide, the content of calcium cyanamide in the lime nitrogen is 61%;
the catalyst is one of aluminum oxide or aluminum silicate;
The method comprises the steps of generating a flame retardant, continuously heating melamine feed liquid to 160-170 ℃ in a high-pressure container, controlling the pressure in the high-pressure container to 0.60-0.71 Mpa, preserving heat for 2.5-3.5 h to obtain melamine cyanurate feed liquid, cooling to 10-20 ℃, preserving heat for 0.5-1.5 h at 10-20 ℃, and performing suction filtration, hot water washing and drying to obtain melamine cyanurate products.
2. The method for preparing a flame retardant using an amine-based waste mother liquor according to claim 1, wherein the content of the cyanamide in the filtrate B is 3.1 to 3.4% in the produced cyanamide.
3. The method for preparing a flame retardant using an amine-based waste mother liquor according to claim 1, wherein in the step of generating the cyanamide, the acidic substance is one of carbon dioxide and sulfuric acid, and when the acidic substance is carbon dioxide, the introducing speed of carbon dioxide is 5mL/min.
4. The method for preparing a flame retardant by utilizing amine waste mother liquor according to claim 1, wherein the weight ratio of the waste mother liquor to the concentrated solution A in the process of generating the cyanamide is 600:300;
In the produced cyanamide, the weight ratio of the drinking water to the lime nitrogen is 200:20.
5. The method for preparing a flame retardant by using an amine-based waste mother liquor according to claim 1, wherein the melamine content in the melamine-based feed solution is 6.4-6.6%.
6. The method for preparing a flame retardant by utilizing an amine-based waste mother liquor according to claim 1, wherein the weight ratio of the concentrated solution A to lime nitrogen in the melamine production is 300:20;
In the melamine production, the mass volume ratio of the concentrated solution A to the drinking water to the catalyst is 300g:200 mL:0.1-0.2 g.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936211A (en) * | 2012-11-13 | 2013-02-20 | 宁夏宝马化工集团有限公司 | Method for continuously producing dicyandiamide |
| CN114751869A (en) * | 2022-04-21 | 2022-07-15 | 山东泰星新材料股份有限公司 | Preparation method of high-dispersion melamine cyanurate flame retardant |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936211A (en) * | 2012-11-13 | 2013-02-20 | 宁夏宝马化工集团有限公司 | Method for continuously producing dicyandiamide |
| CN114751869A (en) * | 2022-04-21 | 2022-07-15 | 山东泰星新材料股份有限公司 | Preparation method of high-dispersion melamine cyanurate flame retardant |
Non-Patent Citations (1)
| Title |
|---|
| Barbara Ju¨rgens等.Melem (2,5,8-Triamino-tri-s-triazine), an Important Intermediate during Condensation of Melamine Rings to Graphitic Carbon Nitride: Synthesis, Structure Determination by X-ray Powder Diffractometry, Solid-State NMR, and Theoretical Studies.《J. AM. CHEM. SOC.》.2003,第125卷(第34期),10288-10300. * |
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