CN103896813A - High-purity dicyandiamide production process - Google Patents
High-purity dicyandiamide production process Download PDFInfo
- Publication number
- CN103896813A CN103896813A CN201410141975.6A CN201410141975A CN103896813A CN 103896813 A CN103896813 A CN 103896813A CN 201410141975 A CN201410141975 A CN 201410141975A CN 103896813 A CN103896813 A CN 103896813A
- Authority
- CN
- China
- Prior art keywords
- filtering
- phase
- liquid filtration
- filter
- secondary liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 title abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 63
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 5
- MYFXBBAEXORJNB-UHFFFAOYSA-N calcium cyanamide Chemical compound [Ca+2].[N-]=C=[N-] MYFXBBAEXORJNB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000002425 crystallisation Methods 0.000 claims abstract description 5
- 230000008025 crystallization Effects 0.000 claims abstract description 5
- 150000002357 guanidines Chemical class 0.000 claims abstract description 5
- 230000007062 hydrolysis Effects 0.000 claims abstract description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 5
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000004744 fabric Substances 0.000 claims abstract description 4
- 239000012528 membrane Substances 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 35
- 238000000926 separation method Methods 0.000 claims description 4
- 235000011089 carbon dioxide Nutrition 0.000 claims description 3
- 238000002386 leaching Methods 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 239000003814 drug Substances 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 239000007791 liquid phase Substances 0.000 abstract 8
- 239000012071 phase Substances 0.000 abstract 3
- 229920000877 Melamine resin Polymers 0.000 abstract 1
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract 1
- 239000001569 carbon dioxide Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000006471 dimerization reaction Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- -1 electronics Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a high-purity dicyandiamide production process. The high-purity dicyandiamide production process comprises lime nitrogen hydrolysis, carbon dioxide decalcification, cyanamide polymerization, filtering, cooling, crystallization, separating and drying, wherein the filtering specifically refers to three-level filtering including primary liquid-phase filtering, secondary liquid-phase filtering and homogeneous-phase filtering; filer cloth of a primary liquid-phase filter is 120 meshes and primary liquid-phase filtering is carried out once at 68 DEG C-73 DEG C to filter out large particles with particle size being greater than 0.1mm; the filter medium of the secondary liquid-phase filter is diatomite and secondary liquid-phase filtering is carried out once at 68 DEG C-73 DEG C to filter out the particles with particle size being greater than 0.01mm; and a homogeneous-phase filter is a multi-level membrane filter which is used for filtering out secondary liquid-phase filtering residue, as well as guanidines, salts and melamine in the liquor, at 68 DEG C-73 DEG C under pressure of 2kg. According to the process, impurities in dicyandiamide liquor can be effectively filtered out by the double liquid-phase filtration and the primary homogeneous-phase filtration, so that the final product can reach the medicine-level requirements.
Description
technical field:
The present invention relates to industry synthetic Dyhard RU 100 technical field, particularly a kind of high purity Dyhard RU 100 production technique.
background technology:
Cyanamid dimerization (abbreviation DICY or DCD) molecular formula is (NH
2cN)
2, have another name called Dyhard RU 100, dicyan diamino, be a kind of white prismatic crystalline powder.Dyhard RU 100 is a kind of important fine chemical material, can be used for medicine, dyestuff, coating, agricultural chemicals, electronics, glass fibre, lubricant and fire retardant etc.Industrial production Dyhard RU 100 is that (molecular formula is C by lime nitrogen
acN
2) hydrolysis, decalcification reaction and filter and obtain cyanamide (molecular formula is NH
2cN) liquid, then carries out cyanamide polymerization, filtration, cooling, crystallization, separation, the dry Dyhard RU 100 product that obtains.Its reaction equation is as follows:
2C
aCN
2+2H
2O?→?C
a?(HCN
2)
2+C
a(OH)
2
C
a(HCN
2)
2+CO
2+H
2O?→?2NH
2CN+C
aCO
3
2NH
2CN?→?(NH
2CN)
2
In many application of Dyhard RU 100, pharmaceutical grade Dyhard RU 100 value of the product is the highest, require also strict, to the by product of building-up process, as guanidine class thing, salt, trimeric cyanamide have strict restriction, conventional synthesis and production process does not reach the index request of pharmaceutical grade Dyhard RU 100.
summary of the invention:
Given this, be necessary to design a kind of high purity Dyhard RU 100 production technique of pharmaceutical grade.
A kind of high purity Dyhard RU 100 production technique, comprising: lime nitrogen hydrolysis, carbonic acid gas decalcification, cyanamide polymerization, filtration, cooling, crystallization, separation, be dried; Be filtered into three-stage filtration, comprise: one-level liquid filtration, secondary liquid filtration, homogeneous phase filter; Wherein:
The present invention filters the impurity thing in effective filtering Dyhard RU 100 solution by twin-stage liquid filtration and one-level homogeneous phase, makes the finished product reach the requirement of pharmaceutical grade.
embodiment:
A kind of high purity Dyhard RU 100 production technique, comprising: lime nitrogen hydrolysis, carbonic acid gas decalcification, cyanamide polymerization, filtration, cooling, crystallization, separation, be dried; Be filtered into three-stage filtration, comprise: one-level liquid filtration, secondary liquid filtration, homogeneous phase filter; Wherein:
secondary liquid filtration: the solution after one-level liquid filtration is pumped to secondary liquid filtration device, secondary liquid filtration device filtration medium is diatomite, filters one time at 68 ~ 73 ℃, particle diameter is greater than to the particulate leaching of 0.01mm;
Claims (1)
1. a high purity Dyhard RU 100 production technique, comprising: lime nitrogen hydrolysis, carbonic acid gas decalcification, cyanamide polymerization, filtration, cooling, crystallization, separation, dry; It is characterized in that: be filtered into three-stage filtration, comprise: one-level liquid filtration, secondary liquid filtration, homogeneous phase filter; Wherein:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410141975.6A CN103896813B (en) | 2014-04-10 | 2014-04-10 | Dyhard RU 100 production technique |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410141975.6A CN103896813B (en) | 2014-04-10 | 2014-04-10 | Dyhard RU 100 production technique |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103896813A true CN103896813A (en) | 2014-07-02 |
| CN103896813B CN103896813B (en) | 2015-09-30 |
Family
ID=50988438
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410141975.6A Expired - Fee Related CN103896813B (en) | 2014-04-10 | 2014-04-10 | Dyhard RU 100 production technique |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103896813B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112209857A (en) * | 2020-10-29 | 2021-01-12 | 宁夏蓝白黑循环科技有限公司 | Preparation method of dicyandiamide |
| CN112457220A (en) * | 2020-10-26 | 2021-03-09 | 石嘴山市鹏盛化工有限公司 | One-step process for producing electronic grade dicyandiamide |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0347045A1 (en) * | 1988-05-18 | 1989-12-20 | Nippon Carbide Kogyo Kabushiki Kaisha | Process for producing cyanamide from calcium cyanamide |
| JPH03157358A (en) * | 1989-11-16 | 1991-07-05 | Nippon Carbide Ind Co Inc | Production of o-methylisourea salt |
| JP2000204007A (en) * | 1999-01-12 | 2000-07-25 | Shinetsu Kasei Kk | Aqueous solution of cyanamide |
| CN101016151A (en) * | 2006-08-08 | 2007-08-15 | 芮海平 | Method for producing cyanamide aqueous solution and dicyandiamide and coproducing carbon and calcium carbonate by using lime nitrogen |
| 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 |
-
2014
- 2014-04-10 CN CN201410141975.6A patent/CN103896813B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0347045A1 (en) * | 1988-05-18 | 1989-12-20 | Nippon Carbide Kogyo Kabushiki Kaisha | Process for producing cyanamide from calcium cyanamide |
| JPH03157358A (en) * | 1989-11-16 | 1991-07-05 | Nippon Carbide Ind Co Inc | Production of o-methylisourea salt |
| JP2000204007A (en) * | 1999-01-12 | 2000-07-25 | Shinetsu Kasei Kk | Aqueous solution of cyanamide |
| CN101016151A (en) * | 2006-08-08 | 2007-08-15 | 芮海平 | Method for producing cyanamide aqueous solution and dicyandiamide and coproducing carbon and calcium carbonate by using lime nitrogen |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 马春庭: "水解连续化新工艺在双氰胺生产中的应用", 《化学工程》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112457220A (en) * | 2020-10-26 | 2021-03-09 | 石嘴山市鹏盛化工有限公司 | One-step process for producing electronic grade dicyandiamide |
| CN112209857A (en) * | 2020-10-29 | 2021-01-12 | 宁夏蓝白黑循环科技有限公司 | Preparation method of dicyandiamide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103896813B (en) | 2015-09-30 |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150930 Termination date: 20200410 |
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| CF01 | Termination of patent right due to non-payment of annual fee |