CN100338116C - Polyamide 1010 resin production process - Google Patents
Polyamide 1010 resin production process Download PDFInfo
- Publication number
- CN100338116C CN100338116C CNB2005100942615A CN200510094261A CN100338116C CN 100338116 C CN100338116 C CN 100338116C CN B2005100942615 A CNB2005100942615 A CN B2005100942615A CN 200510094261 A CN200510094261 A CN 200510094261A CN 100338116 C CN100338116 C CN 100338116C
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- CN
- China
- Prior art keywords
- resin
- polyamide
- water
- sebacic acid
- molecular weight
- 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.)
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- 229920006152 PA1010 Polymers 0.000 title claims abstract description 18
- 239000011347 resin Substances 0.000 title claims abstract description 18
- 229920005989 resin Polymers 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title description 4
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000005516 engineering process Methods 0.000 claims abstract description 16
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 10
- 239000003960 organic solvent Substances 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 8
- YQLZOAVZWJBZSY-UHFFFAOYSA-N decane-1,10-diamine Chemical compound NCCCCCCCCCCN YQLZOAVZWJBZSY-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005453 pelletization Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 239000003112 inhibitor Substances 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical group CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical group C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 2
- QFGCFKJIPBRJGM-UHFFFAOYSA-N 12-[(2-methylpropan-2-yl)oxy]-12-oxododecanoic acid Chemical compound CC(C)(C)OC(=O)CCCCCCCCCCC(O)=O QFGCFKJIPBRJGM-UHFFFAOYSA-N 0.000 claims 1
- 238000006116 polymerization reaction Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000009987 spinning Methods 0.000 abstract description 2
- 239000003973 paint Substances 0.000 abstract 1
- 238000006068 polycondensation reaction Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- TVIDDXQYHWJXFK-UHFFFAOYSA-N dodecanedioic acid Chemical compound OC(=O)CCCCCCCCCCC(O)=O TVIDDXQYHWJXFK-UHFFFAOYSA-N 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 208000005156 Dehydration Diseases 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- SYECJBOWSGTPLU-UHFFFAOYSA-N hexane-1,1-diamine Chemical compound CCCCCC(N)N SYECJBOWSGTPLU-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Abstract
The present invention relates to technology for preparing polyamide 1010 resin, particularly to technology for preparing polyamide 1010 resin by using water as a main body solvent under the technological condition that an organic solvent is not used, or a small amount of organic solvent is used. The technology has the technical scheme that a certain amount of water, sebacic acid, decanediamine, a molecular weight regulator and an auxiliary agent thereof are added into a polymerization kettle, or the polyamide 1010 resin is prepared by polycondensation, or a certain amount of water, sebacic acid, decanediamine, a molecular weight regulator and an auxiliary agent thereof are added into a low pressure container, and are pressed into the polymerization kettle to be prepared into the polyamide 1010 resin after being heated to 100 to 150 DEG C in an anoxybiotic mode. The application of the present invention simplifies a technological flow, and raw material consumption is greatly lowered. The yield of a product is enhanced, and a safety factor is increased. The polyamide 1010 resin prepared by the present invention can be widely applied to the industries of a war industry, machinery, electric wires and cables, an automobile industry, spinning, paint, etc., and can be compared with a product prepared by the traditional technology.
Description
Technical field
The present invention relates to a class and make the technology of polyamide 1010 resin.
Background technology
The polyamide 1010 resin conventional fabrication processes is carried out in two steps: makes salt and polymerization, and in making the salt process, needs to consume a large amount of organic solvents, higher relatively, the secure context requirement strictness especially of main raw material consumption, and with regard to overall craft, relative complex.
Summary of the invention
The object of the present invention is to provide a class to make the technology of polyamide 1010 resin, this technology be do not use or a small amount of with an organic solvent processing condition under and to change with water be that the main body solvent is made polyamide 1010 resin, to cut down the consumption of raw materials, simplify technical process.
Technical scheme of the present invention is as follows:
1. do not use or with an organic solvent change with water on a small quantity and be the main body solvent;
2.A. in polymeric kettle, add quantitative pure water, sebacic acid, decamethylene diamine, molecular weight regulator and auxiliary agent thereof, be warming up to 100-120 ℃, early stage, normal pressure was 1-6 hour, be warming up to 240-265 ℃ again, pressure is less than 1.5Mpa, time 6-10 hour, after question response finished, pelletizing got the finished product polyamide 1010 resin; Or
B. in low pressure vessel, add after quantitative pure water, sebacic acid, decamethylene diamine, molecular weight regulator and the auxiliary agent thereof, anoxybiotic heats up, maintain within the 100-150 ℃ of scope, after be pressed in the polymeric kettle, temperature is controlled at 240-265 ℃, and pressure is less than 1.5Mpa, time 6-10 hour, after question response finished, pelletizing got the finished product polyamide 1010 resin;
3. above-mentioned each weight of material umber proportioning is as follows:
Water 20-150
Sebacic acid, decamethylene diamine total amount 100
Molecular weight regulator 0.01-0.5
Auxiliary agent 0.01-0.8
4. be under the condition of solvent with water, allowing to add organic solvent, comprising methyl alcohol or ethanol.
Described water is preferably distilled water, is ionized water secondly, but influential slightly to quality.The purpose of water can reduce production costs by a relatively large margin, improves safety coefficient.
Described sebacic acid, decamethylene diamine purity are high more, and it is good more to make product quality, and the desirable existence form of its states of matter: sebacic acid is that particulate state, decamethylene diamine are sheet, and is with respect to technical scheme A, very convenient in operation.
Mol ratios such as described sebacic acid and decamethylene diamine are, institute's water consumption accounts for the 20-150% of both total amounts, even scope is wideer, and I haven't seen you for ages influences quality, can increase energy consumption too much.
Described molecular weight regulator is acetate, hexanodioic acid, sebacic acid, dodecanedioic acid etc., or hexanediamine, decamethylene diamine etc., and it is different that its ratio is looked material viscosity.Purpose is to reach the controlling polymers molecular weight for chainpropagation is stopped.
Described auxiliary agent can be phosphorous acid, 1010 oxidation inhibitor etc.Purpose is to prevent the polymkeric substance oxidation.
Two kinds of polymerization processs of described A, B, only different on feeding mode, with regard to its essence, be consistent.
Adopt technology of the present invention, do not have obvious salification process, simplify technical process greatly.
Adopt technology of the present invention, principal character is to do solvent with water, allows to add organic solvent such as methyl alcohol, ethanol etc.A small amount of solvent exists without prejudice to essence of the present invention.
Embodiment
Be described further with a specific examples below:
In polymeric kettle, inject the 40Kg pure water, add 30Kg sebacic acid, 25Kg decamethylene diamine, 12g oxidation inhibitor again, be warming up to 100 ℃ of dehydrations, early stage, normal pressure was 4 hours, was warming up to 250 ℃ more gradually, and pressure is less than 1.5Mpa, 6 hours time, after question response finished, pelletizing got the finished product polyamide 1010 resin.
The polyamide 1010 resin that adopts the present invention to produce is widely used in industries such as military project, machinery, electric wire, automotive industry, spinning, coating, can make product with traditional technology and compare favourably.
Facts have proved that application of the present invention has reduced organic solvent and raw material consumption significantly, has improved product yield, simplified technical process, in operation, bring great convenience, improved production efficiency.
Claims (4)
1. make the technology of polyamide 1010 resin, it is characterized in that:
(1) do not use or with an organic solvent change with water on a small quantity and be the main body solvent;
(2) A. adds quantitative pure water, sebacic acid, decamethylene diamine, molecular weight regulator and auxiliary agent thereof in polymeric kettle, intensification 100-120 ℃, early stage, normal pressure was 1-6 hour, be warming up to 240-265 ℃ again, pressure is less than 1.5Mpa, time 6-10 hour, after question response finished, pelletizing got the finished product polyamide 1010 resin; Or
B. in low pressure vessel, add after quantitative pure water, sebacic acid, decamethylene diamine, molecular weight regulator and the auxiliary agent thereof, anoxybiotic heats up, maintain within the 100-150 ℃ of scope, after be pressed in the polymeric kettle, temperature is controlled at 240-265 ℃, and pressure is less than 1.5Mpa, time 6-10 hour, after question response finished, pelletizing got the finished product polyamide 1010 resin;
(3) above-mentioned each weight of material umber proportioning is as follows:
Water 20-150
Sebacic acid, decamethylene diamine total amount 100
Molecular weight regulator 0.01-0.5
Auxiliary agent 0.01-0.8
(4) be under the condition of solvent with water, allowing to add organic solvent, comprising methyl alcohol or ethanol.
2. the technology described in claims 1 is characterized in that: sebacic acid and decamethylene diamine such as are at mol ratio.
3. the technology described in claims 1 is characterized in that: molecular weight regulator can be acetate or hexanodioic acid, sebacic acid, dodecanedioic acid, and it is different that its consumption is looked material viscosity.
4. the technology described in claims 1, it is characterized in that: auxiliary agent is phosphorous acid or 1010 oxidation inhibitor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100942615A CN100338116C (en) | 2005-09-07 | 2005-09-07 | Polyamide 1010 resin production process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100942615A CN100338116C (en) | 2005-09-07 | 2005-09-07 | Polyamide 1010 resin production process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1737036A CN1737036A (en) | 2006-02-22 |
| CN100338116C true CN100338116C (en) | 2007-09-19 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100942615A Active CN100338116C (en) | 2005-09-07 | 2005-09-07 | Polyamide 1010 resin production process |
Country Status (1)
| Country | Link |
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| CN (1) | CN100338116C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104129009B (en) * | 2013-05-01 | 2018-07-03 | 英威达纺织（英国）有限公司 | For producing the casting of the polyamide of uniform particle |
| CN106866958A (en) * | 2015-12-10 | 2017-06-20 | 上海杰事杰新材料(集团)股份有限公司 | A kind of Long carbon chain amorphous nylon PA1111 materials and preparation method thereof |
| CN113045749B (en) * | 2021-04-15 | 2022-01-28 | 河南华盈新材料有限公司 | Synthesis method of long carbon chain polyamide material |
| CN116041694A (en) * | 2022-12-27 | 2023-05-02 | 无锡殷达尼龙有限公司 | Preparation method for improving oxidation resistance of polyamide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1580094A (en) * | 2003-08-07 | 2005-02-16 | 上海杰事杰新材料股份有限公司 | Process for producing long carbon chain nylon salt |
-
2005
- 2005-09-07 CN CNB2005100942615A patent/CN100338116C/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1580094A (en) * | 2003-08-07 | 2005-02-16 | 上海杰事杰新材料股份有限公司 | Process for producing long carbon chain nylon salt |
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| Publication number | Publication date |
|---|---|
| CN1737036A (en) | 2006-02-22 |
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Effective date of registration: 20140902 Address after: 214183 jade Town, Huishan District, Jiangsu, Wuxi Patentee after: Wuxi Yinda Nylon Co., Ltd. Address before: 214183 jade Town, Huishan District, Jiangsu, Wuxi Patentee before: Dupont Xingda Filaments Co., Ltd. |
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Denomination of invention: Polyamide 1010 resin production process Effective date of registration: 20140911 Granted publication date: 20070919 Pledgee: Wuxi rural commercial bank Limited by Share Ltd Pledgor: Wuxi Yinda Nylon Co., Ltd. Registration number: 2014990000750 |
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Date of cancellation: 20170825 Granted publication date: 20070919 Pledgee: Wuxi rural commercial bank Limited by Share Ltd Pledgor: Wuxi Yinda Nylon Co., Ltd. Registration number: 2014990000750 |
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Denomination of invention: Polyamide 1010 resin production process Effective date of registration: 20170825 Granted publication date: 20070919 Pledgee: Wuxi rural commercial bank Limited by Share Ltd Pledgor: Wuxi Yinda Nylon Co., Ltd. Registration number: 2017990000795 |
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Date of cancellation: 20200827 Granted publication date: 20070919 Pledgee: Wuxi rural commercial bank Limited by Share Ltd. Pledgor: WUXI YINDA NYLON Co.,Ltd. Registration number: 2017990000795 |