CN1616508A - Process for preparing still release agent - Google Patents
Process for preparing still release agent Download PDFInfo
- Publication number
- CN1616508A CN1616508A CN 200410064771 CN200410064771A CN1616508A CN 1616508 A CN1616508 A CN 1616508A CN 200410064771 CN200410064771 CN 200410064771 CN 200410064771 A CN200410064771 A CN 200410064771A CN 1616508 A CN1616508 A CN 1616508A
- Authority
- CN
- China
- Prior art keywords
- release agent
- preparation
- still release
- solution
- still
- 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
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- 238000004519 manufacturing process Methods 0.000 title abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 30
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 239000000243 solution Substances 0.000 claims description 21
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 150000004782 1-naphthols Chemical class 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000004202 carbamide Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N aminothiocarboxamide Natural products NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 5
- -1 thiourea peroxide Chemical class 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 3
- 239000007859 condensation product Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000006068 polycondensation reaction Methods 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 2
- 239000004800 polyvinyl chloride Substances 0.000 abstract description 10
- 239000011347 resin Substances 0.000 abstract description 10
- 229920005989 resin Polymers 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 6
- 229920000915 polyvinyl chloride Polymers 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 2
- 238000004040 coloring Methods 0.000 abstract description 2
- 230000001603 reducing effect Effects 0.000 abstract description 2
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical compound C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 abstract 2
- RYYXDZDBXNUPOG-UHFFFAOYSA-N 4,5,6,7-tetrahydro-1,3-benzothiazole-2,6-diamine;dihydrochloride Chemical compound Cl.Cl.C1C(N)CCC2=C1SC(N)=N2 RYYXDZDBXNUPOG-UHFFFAOYSA-N 0.000 abstract 1
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 239000003712 decolorant Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 2
- 238000012356 Product development Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- HRKQOINLCJTGBK-UHFFFAOYSA-N dihydroxidosulfur Chemical compound OSO HRKQOINLCJTGBK-UHFFFAOYSA-N 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Abstract
The present invention relates to the preparation of chemical product, and especially the preparation process of chemical assistant for polyvinyl chloride resin production. The still release agent is prepared with thiourea dioxide as reducing decolorant and through the condensation of 1-naphthol and formaldehyde under alkali environment. The preparation process is simple and low in cost, and the prepared still release agent has high still releasing capacity and no coloring.
Description
Affiliated technical field
The present invention relates to a kind of preparation technology of Chemicals, particularly a kind of preparation method who is used for the still release agent of polyvinyl chloride resin production.
Background technology
When carrying out the production of Chemicals polyvinyl chloride (PVC) RESINS, generally all in polymerization process, add the polymerization used additives at present.In polymerization process, parts such as the inwall of polymeric kettle, plate washer, still top, stirring rake and condenser all easily produce kettle pasting matter, the kettle pasting matter that produces can pollute resin, cause the increase of black yellow point and flake, the kettle pasting matter of accumulation also can influence the heat transfer of polymeric kettle, strengthen the danger of production process, extended manufacture cycle, caused output to descend.In order to keep ordinary production, must remove the kettle pasting matter of accumulation, clear still process will increase the non-cutting time of producing, and polyvinyl monomer can be to clear still workman's healthy generation harm when adopting artificial clear still, and the while also pollutes the environment.Therefore, inexpensive still release agent is all being sought by each producer when improving production capacity.
Our domestic production producer is in external imported technology and equipment, and the foreign trader tends to require the import still release agent of manufacturer's kitting costliness, has increased production cost.Because still release agent product development degree, the still release agent of domestic production in use still can produce sticking still phenomenon to some extent, cause occurring product defectses such as flake, and influence output.
In addition, owing to still release agent directly contacts with product in the production process of polyvinyl chloride (PVC) RESINS, so the color of still release agent itself also can influence the color of producing the product polyvinyl chloride (PVC) RESINS.As a kind of preparation technology of " 1-naphthols-formaldehyde-alkali " system of the ICI Imperial Chemical Industries of Britain, what obtain is blue or navy blue liquid, and transparency is bad, easily makes polyvinyl chloride (PVC) RESINS painted in process of production.
Studies show that thiourea peroxide is a kind of relatively chemical of safety, resolve into the sulfoxylic acid of urea and strong reducing property in basic solution, is a kind of decolouring reductive agent, uses in printing and dyeing.
Summary of the invention
Ability for the removing kettle pasting matter that strengthens still release agent, overcome the different polyvinyl chloride colorings that make of color simultaneously because of color with the polyvinyl chloride (PVC) RESINS of still release agent, by the preparation technology who improves still release agent, the color that changes still release agent, make itself and polyvinyl chloride (PVC) RESINS color similarity, effectively overcome existing sticking still agent above shortcomings.The present invention is exactly in the preparation technology who improves still release agent, uses the reduction-decolor agent, produces a kind of color xanchromatic still release agent close with the polyvinyl chloride (PVC) RESINS color.
The present invention is used to solve the technical scheme that its technical problem adopts: a kind of preparation method of still release agent, and use thiourea peroxide as the reduction-decolor agent, polycondensation under alkaline environment gets by 1-naphthols and formaldehyde.
Further: described alkaline environment is the NaOH aqueous solution of pH value 11～13.
Further: described temperature of reaction is 65～95 ℃.
Further, have following technical process:
(a) 1-naphthols, water and the NaOH aqueous solution are joined in the reactor, under effectively stirring, mixing solutions is heated;
(b) with sulfurous gas urea solution and the two mixing of formalin, be added drop-wise in the reactor, guarantee to be in the reactor alkaline environment;
(c) under agitation reaction solution is heated up and insulation, continue to add the sulfurous gas urea solution of surplus;
(d) cooling reaction solution adds surfactant soln, water and polyvinyl alcohol solution to reaction solution, regulates solids concn, fully stirs, and obtaining color is light yellow alkaline aqueous solution to yellowish green 1-naphthols and formaldehyde condensation products.
The invention has the advantages that: production technique is simple, and production cost is low, and it is strong that the still release agent by this prepared does not produce painted and antiseized still ability.
Embodiment
A kind of preparation method of still release agent uses thiourea peroxide as the reduction-decolor agent, and polycondensation under alkaline environment gets by 1-naphthols and formaldehyde, and alkaline environment is the NaOH aqueous solution of pH value 11～13, and temperature of reaction is 65～95 ℃.
Have technical process:
(a) 10～20 parts of 1-naphthols, 40～150 parts of water and 3～10 parts of content 32%NaOH aqueous solution are joined in the reactor, under effectively stirring, mixing solutions is heated to 70 ℃.
(b) 75～200g concentration 4%w/w sulfurous gas urea solution is divided into two parts, the thiourea peroxide of total amount 30～40% and the two mixing of 37% formalin of 3～10 parts will be accounted for, be added drop-wise in the reactor in 0.5～3 hour, guarantee to be alkaline environment in the reactor, temperature is no more than 85 ℃.
(c) under agitation reaction solution is heated to 87～93 ℃, temperature of reactor is no more than 95 ℃, is incubated 0.5～2 hour, continues to add the sulfurous gas urea solution of surplus when heating up and be incubated.
(d) cooling reaction solution, when being cooled to 65 ℃, the surfactant soln, 1～100% water, 0.1～10% the polyvinyl alcohol solution that add 3～5 part 20% are to reaction solution, and the adjusting solids concn reaches 5～6%.
(e) fully stir, obtain color and be light yellow to yellow-green colour, pH value be 12～13 the 1-naphthols and the alkaline aqueous solution of formaldehyde condensation products.
Claims (5)
1. the preparation method of a still release agent is characterized in that: use thiourea peroxide as the reduction-decolor agent, polycondensation under alkaline environment gets by 1-naphthols and formaldehyde.
2. the preparation method of still release agent according to claim 1, it is characterized in that: described alkaline environment is a pH value 11～13.
3. the preparation method of still release agent according to claim 1, it is characterized in that: described temperature of reaction is 65～95 ℃.
4. the preparation method of still release agent according to claim 1, it is characterized in that: described alkaline environment is the NaOH aqueous solution.
5. the preparation method of still release agent according to claim 1 is characterized in that having following technical process:
(a) 1-naphthols, water and the NaOH aqueous solution are joined in the reactor, under effectively stirring, mixing solutions is heated;
(b) with sulfurous gas urea solution and the two mixing of formalin, be added drop-wise in the reactor, guarantee to be in the reactor alkaline environment;
(c) under agitation reaction solution is heated up and insulation, continue to add the sulfurous gas urea solution of surplus;
(d) cooling reaction solution adds surfactant soln, water and polyvinyl alcohol solution to reaction solution, regulates solids concn, fully stirs, and obtaining color is light yellow alkaline aqueous solution to yellowish green 1-naphthols and formaldehyde condensation products.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410064771 CN1288182C (en) | 2004-09-24 | 2004-09-24 | Process for preparing still release agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410064771 CN1288182C (en) | 2004-09-24 | 2004-09-24 | Process for preparing still release agent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1616508A true CN1616508A (en) | 2005-05-18 |
| CN1288182C CN1288182C (en) | 2006-12-06 |
Family
ID=34764576
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410064771 Expired - Fee Related CN1288182C (en) | 2004-09-24 | 2004-09-24 | Process for preparing still release agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1288182C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104011149A (en) * | 2011-10-12 | 2014-08-27 | 英尼奥斯欧洲股份公司 | Additive, composition comprising it and use thereof |
| CN104629551A (en) * | 2015-02-10 | 2015-05-20 | 河北盛华化工有限公司 | Production method for producing high-impact-resistance polyvinyl chloride resin anti-sticking kettle agent |
-
2004
- 2004-09-24 CN CN 200410064771 patent/CN1288182C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104011149A (en) * | 2011-10-12 | 2014-08-27 | 英尼奥斯欧洲股份公司 | Additive, composition comprising it and use thereof |
| US9434844B2 (en) | 2011-10-12 | 2016-09-06 | Ineos Europe Ag | Additive, composition comprising it and use thereof |
| TWI567090B (en) * | 2011-10-12 | 2017-01-21 | 億諾斯歐洲公司 | Additive, composition comprising it and use thereof |
| CN104011149B (en) * | 2011-10-12 | 2017-05-24 | 英尼奥斯欧洲股份公司 | Additive, composition comprising it and use thereof |
| CN104629551A (en) * | 2015-02-10 | 2015-05-20 | 河北盛华化工有限公司 | Production method for producing high-impact-resistance polyvinyl chloride resin anti-sticking kettle agent |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1288182C (en) | 2006-12-06 |
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| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
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| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: CHANGZHOU WUJIN JIAHUA CHEMICAL Co.,Ltd. Assignor: Xue Hua Contract fulfillment period: 2007.1.1 to 2024.1.1 Contract record no.: 2009320000567 Denomination of invention: Process for preparing still release agent Granted publication date: 20061206 License type: Exclusive license Record date: 20090413 |
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| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2007.1.1 TO 2024.1.1; CHANGE OF CONTRACT Name of requester: CHANGZHOU WUJIN JIAHUA CHEMICAL INDUSTRY CO., LTD. Effective date: 20090413 |
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| ASS | Succession or assignment of patent right |
Owner name: CHANGZHOU WUJINJIAHUA CHEMICAL CO., LTD Free format text: FORMER OWNER: XUE HUA Effective date: 20100806 |
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Free format text: CORRECT: ADDRESS; FROM: 213168 NO.1, LIHU WEST ROAD, LUJIA LANE, NIUTANG TOWN, CHANGZHOU CITY, JIANGSU PROVINCE TO: 213168 NO.19, HUBIN NORTH ROAD, NIUTANG TOWN, WUJIN DISTRICT, CHANGZHOU CITY, JIANGSU PROVINCE |
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| TR01 | Transfer of patent right |
Effective date of registration: 20100806 Address after: 213168, No. 19 Hubin North Road, Niu Tong Town, Wujin District, Jiangsu, Changzhou Patentee after: CHANGZHOU WUJIN JIAHUA CHEMICAL Co.,Ltd. Address before: 213168 Jiangsu city of Changzhou province Niu Tang Zhen Lu Jia Xiang Ge Lake Road No. 1 Patentee before: Xue Hua |
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| C56 | Change in the name or address of the patentee |
Owner name: JIANGSU JIAHUA ADVANCED MATERIALS TECHNOLOGY CO., Free format text: FORMER NAME: JIANGSU WUJIN JIAHUA CHEMICAL CO., LTD. |
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| CP03 | Change of name, title or address |
Address after: 213168 No. 19 Hubin North Road, Wujin hi tech Industrial Development Zone, Changzhou, Jiangsu Patentee after: JIANGSU JIAHUA ADVANCED MATERIALS TECHNOLOGY Co.,Ltd. Address before: 213168, No. 19 Hubin North Road, Niu Tong Town, Wujin District, Jiangsu, Changzhou Patentee before: CHANGZHOU WUJIN JIAHUA CHEMICAL Co.,Ltd. |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20061206 Termination date: 20210924 |
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| CF01 | Termination of patent right due to non-payment of annual fee |