CN103172902A - Method for recycling solvent during poly-para-phenylene terephthalamide reaction - Google Patents
Method for recycling solvent during poly-para-phenylene terephthalamide reaction Download PDFInfo
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- CN103172902A CN103172902A CN2013101406605A CN201310140660A CN103172902A CN 103172902 A CN103172902 A CN 103172902A CN 2013101406605 A CN2013101406605 A CN 2013101406605A CN 201310140660 A CN201310140660 A CN 201310140660A CN 103172902 A CN103172902 A CN 103172902A
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- Prior art keywords
- ppta
- solution
- calcium chloride
- utilization method
- circulation utilization
- Prior art date
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- 239000002904 solvent Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 10
- 238000004064 recycling Methods 0.000 title abstract 3
- 239000001110 calcium chloride Substances 0.000 claims abstract description 20
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 20
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 19
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000004821 distillation Methods 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 3
- 229920003366 poly(p-phenylene terephthalamide) Polymers 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 5
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 239000012452 mother liquor Substances 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- HIKUCVORZZXYNF-UHFFFAOYSA-L calcium;1-methylpyrrolidin-2-one;dichloride Chemical compound Cl[Ca]Cl.CN1CCCC1=O HIKUCVORZZXYNF-UHFFFAOYSA-L 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 238000005374 membrane filtration Methods 0.000 claims description 2
- 235000010216 calcium carbonate Nutrition 0.000 claims 2
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 claims 1
- 229910000020 calcium bicarbonate Inorganic materials 0.000 claims 1
- 235000011116 calcium hydroxide Nutrition 0.000 claims 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims 1
- 239000000292 calcium oxide Substances 0.000 claims 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims 1
- 235000012255 calcium oxide Nutrition 0.000 claims 1
- 230000007935 neutral effect Effects 0.000 claims 1
- 230000003472 neutralizing effect Effects 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 6
- 238000005265 energy consumption Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 3
- 238000010612 desalination reaction Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- AVQQQNCBBIEMEU-UHFFFAOYSA-N 1,1,3,3-tetramethylurea Chemical compound CN(C)C(=O)N(C)C AVQQQNCBBIEMEU-UHFFFAOYSA-N 0.000 description 1
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- GNOIPBMMFNIUFM-UHFFFAOYSA-N hexamethylphosphoric triamide Chemical compound CN(C)P(=O)(N(C)C)N(C)C GNOIPBMMFNIUFM-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to a method for recycling a solvent during poly-para-phenylene terephthalamide reaction, and belongs to the technical field of synthesis of high-molecular materials. The poly-para-phenylene terephthalamide prepared through polycondensation at a low temperature is washed to obtain an NMP (N-Methylpyrrolidone) and calcium chloride water solution, and the NMP and calcium chloride water solution passes through a filtering system, a dewatering system, a coarse distillation system, a preparation system, a fine distillation system, and the like to obtain an NMP-calcium chloride solution with water ratio less than 150 ppm. The method disclosed by the invention reduces the operating temperature and enhances the solution purity by adding an auxiliary agent to the coarse distillation system, obtains an NMP-calcium chloride system capable of being recycled in a polymerization unit through the preparation system and solves the problem of recycling of calcium chloride.
Description
Technical field
The present invention relates to the circulation utilization method of solvent in a kind of PPTA reaction, belong to the synthesis of polymer material technical field.
Background technology
PPTA (PPTA) is a kind of high-performance engineering material, can select hexamethylphosphoramide, N,N-DIMETHYLACETAMIDE, N-Methyl pyrrolidone and tetramethyl-urea etc. as solvent in building-up process, wherein N-Methyl pyrrolidone (NMP) is widely used.NMP is expensive, in building-up process, and NMP usage quantity large and strict (such as requiring water ratio＜150ppm etc.), thereby recycled solvent is one of key factor that reduces PPTA cost and industrialization.In synthetic PPTA process, often use calcium chloride as solubility promoter, yet the recycle of calcium chloride is still open question now.
Understand according to the applicant, application number is 200610037771.3, the Chinese patent that name is called " circulation utilization method of polymer solvent in the PPTA building-up reactions " discloses the circulation utilization method of solvent in the PPTA building-up reactions, wherein need to carry out the step of desalination, because the demineralising process energy consumption is large, and salt can't recycle, and therefore can't avoid waste.Application number is the patent of 200810225081.X, discloses a kind of method that adopts the aromatic series extraction agent to reclaim nmp solvent, although the method has reduced service temperature, the extraction agent severe toxicity therefore not only have danger, and use cost increases.Application number is 200710039497.8 patent, adopts thin-film evaporator that the water in solution and NMP are steamed, and calcium chloride is difficult to recycle, and energy consumption is larger.
Summary of the invention
The technical problem to be solved in the present invention is the defective that exists for prior art, proposes the circulation utilization method of solvent in a kind of PPTA reaction.
The present invention is the technical solution problem by the following technical programs, and the circulation utilization method of solvent in a kind of PPTA reaction comprises the following steps:
Step 1, the PPTA that low-temperature polycondensation is obtained are washed, and obtain washings;
Step 2, washings is neutralized obtains neutralizer;
Step 3, described neutralizer is removed by filter impurity, obtain containing the solution of N-Methyl pyrrolidone, calcium chloride and water, as mother liquor;
Step 4, described mother liquor dewaters, slightly heats up in a steamer, solution preparation, rectifying obtain water-content≤150ppm N-Methyl pyrrolidone-calcium chloride solvent system is carried out recycle.
Wherein, be filtered at least a in bag type filtering, membrane filtration and tubular filter in described step 3, filtering accuracy is 0.1-20um.
In described step 4, with the underpressure distillation dehydration, pounds per square inch absolute (psia) is 2-5KPa, and temperature is 60-90 ℃.
Described slightly heating up in a steamer is slightly to heat up in a steamer in topping still, pounds per square inch absolute (psia) 0.1-3KPa in tower, and temperature is 50-110 ℃.Add at least a as auxiliary agent in methyl alcohol, ethanol, ethylene glycol in slightly heating up in a steamer process.Described promoter addition is the 0.1%-2% of solution quality.
Described solution preparation is to add Calcium Chloride Powder Anhydrous or NMP in through the solution after slightly heating up in a steamer step, obtains the solution that calcium chloride concentration is 0.1-0.2mol/L.
Described rectifying is to carry out rectifying in distilling filled tower, and the pounds per square inch absolute (psia) of distilling filled tower is 0.1-2KPa, and temperature is 50-110 ℃.
Advantage of the present invention is as follows: 1. increase filtering system, improve the solution cleanliness factor; 2. add auxiliary agent in slightly heating up in a steamer process, reduce service temperature, reduce energy consumption, and improve overhead product purity; 3. save the desalination step, realize that calcium chloride reclaims use, reduces energy consumption; 4. do not contain highly toxic substance, through engineering approaches safety and reliability in technique; 5. solvent recovering rate is high, reaches 97%.
Description of drawings
Fig. 1 is the schematic flow sheet of the embodiment of the present invention.
Embodiment
Embodiment one
The present embodiment carries out recycle by following steps to solvent: add calcium hydroxide to obtain the neutralizer of pH=7 in washings, neutralizer is passed through deep bed filter, filtering accuracy 5um, collect filtered liquid in storage tank, filtered liquid is sent into dewatering system carry out the underpressure distillation dehydration, distillation parameter pounds per square inch absolute (psia) 2KPa, temperature is 70 ℃, dewatering system can be removed most of water.Then add 2% ethanol auxiliary agent in the solution, and solution is sent into the system of slightly heating up in a steamer, control pounds per square inch absolute (psia) 3KPa in topping still, temperature is 90 ℃, slightly heats up in a steamer water ratio in rear solution＜0.5%.Add Calcium Chloride Powder Anhydrous to slightly heating up in a steamer in rear solution, obtain the solution that calcium chloride concentration is 0.13mol/L, solution is inputted rectifying tower, in tower, pounds per square inch absolute (psia) is 0.2KPa, and temperature is 80 ℃.Through after rectifying, obtaining water ratio is the NMP-calcium chloride solution of 150ppm, and this solution can be input to polymerized unit, uses as the solvent cycle of polyreaction.Wherein the NMP rate of recovery 97.5%.
Embodiment two
The present embodiment carries out recycle by following steps to solvent: add calcium carbonate to obtain the neutralizer of pH=7 in washings, neutralizer is passed through pipe filter, filtering accuracy 3um, collect filtered liquid in storage tank, filtered liquid is sent into dewatering system carry out the underpressure distillation dehydration, distillation parameter pounds per square inch absolute (psia) 3KPa, temperature is 90 ℃.Then add 0.5% ethanol-methyl alcohol auxiliary agent in the solution, and solution is sent into the system of slightly heating up in a steamer, control pounds per square inch absolute (psia) 2KPa in topping still, temperature is 100 ℃, slightly heats up in a steamer water ratio in rear solution＜0.3%.Add Calcium Chloride Powder Anhydrous to slightly heating up in a steamer in rear solution, obtain the solution that calcium chloride concentration is 0.15mol/L, solution is inputted rectifying tower, in tower, pounds per square inch absolute (psia) is 1.5KPa, and temperature is 110 ℃.Through after rectifying, obtaining water ratio is the NMP-calcium chloride solution of 110ppm, and this solution can be input to polymerized unit, uses as the solvent cycle of polyreaction.Wherein the NMP rate of recovery 98.0%.
Embodiment three
The present embodiment carries out recycle by following steps to solvent: add calcium hydroxide to obtain the neutralizer of pH=7 in washings, neutralizer is passed through deep bed filter, filtering accuracy 2um, collect filtered liquid in storage tank, filtered liquid is sent into dewatering system carry out the underpressure distillation dehydration, distillation parameter pounds per square inch absolute (psia) 4KPa, temperature is 80 ℃.Then add 1% methyl alcohol auxiliary agent in the solution, and solution is sent into the system of slightly heating up in a steamer, control pounds per square inch absolute (psia) 1KPa in topping still, temperature is 80 ℃, slightly heats up in a steamer water ratio in rear solution＜0.8%.Add Calcium Chloride Powder Anhydrous to slightly heating up in a steamer in rear solution, obtain the solution that calcium chloride concentration is 0.17mol/L, solution is inputted rectifying tower, in tower, pounds per square inch absolute (psia) is 0.8KPa, and temperature is 100 ℃.Through after rectifying, obtaining water ratio is the NMP-calcium chloride solution of 120ppm, and this solution can be input to polymerized unit, uses as the solvent cycle of polyreaction.Wherein the NMP rate of recovery 97%.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.
Claims (9)
1. the circulation utilization method of solvent during a PPTA is reacted comprises the following steps:
Step 1, the PPTA that low-temperature polycondensation is obtained are washed, and obtain washings;
Step 2, washings is neutralized obtains neutralizer;
Step 3, described neutralizer is removed by filter impurity, obtain containing the solution of N-Methyl pyrrolidone, calcium chloride and water, as mother liquor;
Step 4, described mother liquor dewaters, slightly heats up in a steamer, solution preparation, rectifying obtain water-content≤150ppm N-Methyl pyrrolidone-calcium chloride solvent system is carried out recycle.
2. the circulation utilization method of solvent during PPTA is reacted according to claim 1, it is characterized in that: in described step 2, neutralizing agent is at least a in calcium hydroxide, calcium oxide, calcium carbonate, Calcium hydrogen carbonate, is neutralized to solution and is neutral.
3. the circulation utilization method of solvent in PPTA reaction according to claim 1 is characterized in that: be filtered at least a in bag type filtering, membrane filtration, tubular filter in described step 3, filtering accuracy is 0.1-20um.
4. the circulation utilization method of solvent during PPTA is reacted according to claim 1 is characterized in that: in described step 4, with the underpressure distillation dehydration, pounds per square inch absolute (psia) is 2-5KPa, and temperature is 60-100 ℃.
5. the circulation utilization method of solvent during PPTA is reacted according to claim 4 is characterized in that: slightly heats up in a steamer in topping still, and pounds per square inch absolute (psia) 0.1-3KPa in tower, temperature is 50-110 ℃.
6. the circulation utilization method of solvent in PPTA reaction according to claim 5 is characterized in that: add at least a as auxiliary agent in methyl alcohol, ethanol, ethylene glycol in slightly heating up in a steamer process.
7. the circulation utilization method of solvent during PPTA is reacted according to claim 6, it is characterized in that: described promoter addition is the 0.1%-2% of solution quality.
8. the circulation utilization method of solvent during PPTA is reacted according to claim 4, it is characterized in that: described solution preparation is to add Calcium Chloride Powder Anhydrous or NMP in through the solution after slightly heating up in a steamer step, obtains the solution that calcium chloride concentration is 0.1-0.2mol/L.
9. the circulation utilization method of solvent during PPTA is reacted according to claim 5, it is characterized in that: carry out rectifying in distilling filled tower, the pounds per square inch absolute (psia) of distilling filled tower is 0.1-2KPa, and temperature is 50-110 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106367827A (en) * | 2016-10-11 | 2017-02-01 | 四川辉腾科技股份有限公司 | Method for washing meta-aramid fibrid |
| CN106565985A (en) * | 2015-10-12 | 2017-04-19 | 中国石化仪征化纤有限责任公司 | Continuous recycling method for solvent in para-aramid polymerization waste |
| CN109134852A (en) * | 2018-09-06 | 2019-01-04 | 南京工业大学 | Method for realizing zero discharge of poly (p-phenylene terephthalamide) filtering and washing wastewater |
| CN113234222A (en) * | 2021-05-17 | 2021-08-10 | 河南神马尼龙化工有限责任公司 | Production device and process of high-quality complexing solvent for PPTA polymerization |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1810851A (en) * | 2006-01-13 | 2006-08-02 | 常熟市贝斯特皮革有限公司 | Polymerizing solution reusing method for polymerization of paraphthaolyl p-phenylenediamine |
| CN101805456A (en) * | 2010-03-16 | 2010-08-18 | 苏州兆达特纤科技有限公司 | Method for reclaiming solvent in poly(p-phenytene terephthalamide)resin production |
-
2013
- 2013-04-19 CN CN201310140660.5A patent/CN103172902B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1810851A (en) * | 2006-01-13 | 2006-08-02 | 常熟市贝斯特皮革有限公司 | Polymerizing solution reusing method for polymerization of paraphthaolyl p-phenylenediamine |
| CN101805456A (en) * | 2010-03-16 | 2010-08-18 | 苏州兆达特纤科技有限公司 | Method for reclaiming solvent in poly(p-phenytene terephthalamide)resin production |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106565985A (en) * | 2015-10-12 | 2017-04-19 | 中国石化仪征化纤有限责任公司 | Continuous recycling method for solvent in para-aramid polymerization waste |
| CN106367827A (en) * | 2016-10-11 | 2017-02-01 | 四川辉腾科技股份有限公司 | Method for washing meta-aramid fibrid |
| CN106367827B (en) * | 2016-10-11 | 2018-06-29 | 四川辉腾科技股份有限公司 | A kind of washing methods of meta-aramid fibre fibrid |
| CN109134852A (en) * | 2018-09-06 | 2019-01-04 | 南京工业大学 | Method for realizing zero discharge of poly (p-phenylene terephthalamide) filtering and washing wastewater |
| CN113234222A (en) * | 2021-05-17 | 2021-08-10 | 河南神马尼龙化工有限责任公司 | Production device and process of high-quality complexing solvent for PPTA polymerization |
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| CN103172902B (en) | 2015-12-09 |
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Address after: 210019 Yunlong road 79, Jianye District, Jiangsu, Nanjing Patentee after: CHINA NUCLEAR HUAWEI ENGINEERING DESIGN AND RESEARCH Co.,Ltd. Address before: 210019 Yunlong road 79, Jianye District, Jiangsu, Nanjing Patentee before: JIANGSU CHINA NUCLEAR INDUSTRY HUAWEI ENGINEERING DESIGN AND RES Co.,Ltd. |
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