CN104877135A - Washing and purifying method for polyphenylene sulfide resin production - Google Patents
Washing and purifying method for polyphenylene sulfide resin production Download PDFInfo
- Publication number
- CN104877135A CN104877135A CN201510298212.7A CN201510298212A CN104877135A CN 104877135 A CN104877135 A CN 104877135A CN 201510298212 A CN201510298212 A CN 201510298212A CN 104877135 A CN104877135 A CN 104877135A
- Authority
- CN
- China
- Prior art keywords
- polyphenylene sulfide
- product
- sulfide resin
- washing
- mixture
- 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.)
- Pending
Links
Abstract
The invention relates to a washing and purifying method for polyphenylene sulfide resin production. The method includes: (1), dissolving hydrogenous sodium sulfide in NMP (N-Methyl pyrrolidone), dehydrating the hydrogenous sodium sulfide through inert gas shielding under the catalytic action of lithium chloride and caustic soda flakes, and adding DCB (dichloro-benzidine) and NMP liquor for polymerization reaction to obtain polyphenylene sulfide resin mixture slurry; (2), performing solid-liquid separation on the polyphenylene sulfide resin mixture slurry to obtain a polyphenylene sulfide resin product containing low polymers, a by-product salt mixture and most of the NMP liquor respectively; (3), subjecting the polyphenylene sulfide resin product containing the low polymers and the by-product salt mixture to reverse soaking and rinsing to obtain a salty coarse polyphenylene sulfide resin product and rinsing liquid respectively; (4), subjecting the salty coarse polyphenylene sulfide resin product to filtering, washing and separating to obtain cleaning liquid and a wet polyphenylene sulfide product respectively, and drying the wet polyphenylene sulfide product to obtain a qualified polyphenylene sulfide resin product. By the washing and purifying method, cost can be reduced and product quality can be guaranteed.
Description
Technical field
The present invention relates to organic polymer resin production technical field, particularly relate to a kind of method of producing polyphenylene sulfide washing, purifying.
Background technology
Adopt sodium sulphite (Na
2sH
2o) with santochlor (P-DCB) be raw material, under basic metal and lithium salts promoter effect, polycondensation is produced in the technological process of polyphenylene sulfide (PPS) resin, in PPS resin, impurities has a strong impact on its use properties, the oligopolymer particularly produced in polymerization process is difficult to be separated, therefore, effectively can be separated, Purification Resin is the gordian technique of producing PPS qualified product.
After completion of the polymerization reaction, method by routine removes the oligopolymer of 70 ~ 75%, but 25 ~ 30% of remainder combine with PPS product, extremely difficult separation, therefore, contained by the PPS resin that traditional industrial method is produced, oligopolymer exceeds standard, and has a strong impact on the performance of PPS product and the application of derived product.
The extraction agent adopting methyl alcohol to be used as extracting oligopolymer, ring compound, NMP solvent and by product alkali metal halide in polyphenylene sulfide is described in United States Patent (USP) number US6437024, this by product should be lithium chloride wherein, and it adopts lithium sulfide to be the starting material that polyphenylene sulfide synthesizes.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method not only having reduced costs but also ensured production polyphenylene sulfide washing that product is qualified, purifying.
For solving the problem, a kind of method of producing polyphenylene sulfide washing, purifying of the present invention, comprises the following steps:
(1) many water cure sodium is dissolved in the solvent NMP of its quality 2.5 ~ 3.5 times, under the katalysis of auxiliary agent lithium chloride and sheet alkali, the moisture in described many water cure sodium is taken off by protection of inert gas, add DCB and nmp solution again, polyreaction is carried out according to a conventional method, synthesis polyphenylene sulfide mixture slip in closed reactor; Described DCB is 0.8 ~ 0.85 times of described many water cure sodium quality, and described nmp solution is 1 ~ 1.5 times of described many water cure sodium quality;
(2) with sleeping spiral shell sedimentation conveyer centrifugal, described polyphenylene sulfide mixture slip is carried out solid-liquid separation, obtain the polyphenylene sulfide resin fat prod containing 5 ~ 10% oligopolymer and the mixture of by-product salt, most of nmp solution respectively;
(3) the mixture of described the polyphenylene sulfide resin fat prod and by-product salt that contain 5 ~ 10% oligopolymer is joined in leacher, and remove oligopolymer in thick product and most of by-product salt with 4 times of reverse immersions of the deionized water to mixture quality, rinsing, obtain the thick product of polyphenylene sulfide and the rinsing liquid of saliferous respectively;
(4) thick for the polyphenylene sulfide of described saliferous product is inputed in the two-in-one strainer of 180 order stainless steel, be separated with the deionized water wash laggard row solid-liquid second stage, remove the by-product salt in polyphenylene sulfide product, obtain scavenging solution and wet polyphenylene sulfide product respectively; Described wet polyphenylene sulfide product obtains qualified polyphenylene sulfide resin fat prod through vacuum-drying.
Described step (2) in the condition of solid-liquid separation refer to that described mixture temperature is 100 ~ 150 DEG C, centrifugal owner's rotating speed is 3000 ~ 3500r/min, and disengaging time is 1 ~ 1.5h.
Described step (3) in the temperature of deionized water be 90 ~ 95 DEG C.
Described step (4) in vacuum drying condition refer to and adopt SGZ double-cone vacuum dryer, its vacuum tightness is-0.05 ~-0.08MPa, and heating low-pressure steam is 3 ~ 5kg, and time of drying is 90 ~ 110 minutes.
The present invention compared with prior art has the following advantages:
1, the present invention adopts the reverse rinsing of leacher, can effectively remove the oligopolymer affecting PPS resin quality, solves PPS resin purification problem in traditional technology, and the oligopolymer namely produced in synthesis is difficult to be separated and has a strong impact on the serious problems of product quality.
2, separation method of the present invention is easy, reliable, to equipment and production environment conditional request low and effectively can reduce PPS production of resins cost.
3, the PPS product whiteness adopting the inventive method to obtain can reach more than 80%, H
2o≤0.3%, impurity≤0.3%, indices all reaches national standard, and even part of standards is better than foreign standard.
Embodiment
embodiment 1produce a method for polyphenylene sulfide washing, purifying, comprise the following steps:
(1) many water cure sodium is dissolved in the solvent NMP(n-methyl-2-pyrrolidone of its quality 2.5 times) in; under the katalysis of auxiliary agent lithium chloride and sheet alkali; the moisture in many water cure sodium is taken off by protection of inert gas; add DCB(santochlor again) and nmp solution; polyreaction is carried out according to a conventional method, synthesis polyphenylene sulfide mixture slip in closed reactor.
Wherein: DCB is 0.8 times of many water cure sodium quality, nmp solution is 1 times of many water cure sodium quality.
(2) with sleeping spiral shell sedimentation conveyer centrifugal, polyphenylene sulfide mixture slip is carried out solid-liquid separation, obtain the polyphenylene sulfide resin fat prod containing 5 ~ 10% oligopolymer and the mixture of by-product salt, most of nmp solution respectively.
Wherein: the condition of solid-liquid separation refers to that mixture temperature is 100 DEG C, and centrifugal owner's rotating speed is 3000r/min, and disengaging time is 1h.
(3) the mixture of the polyphenylene sulfide resin fat prod containing 5 ~ 10% oligopolymer and by-product salt is joined in leacher, and remove oligopolymer in thick product and most of by-product salt with 4 times of reverse immersions of the deionized water to mixture quality, rinsing, obtain the thick product of polyphenylene sulfide and the rinsing liquid of saliferous respectively.
Wherein: the temperature of deionized water is 90 DEG C.
(4) thick for the polyphenylene sulfide of saliferous product is inputed in the two-in-one strainer of 180 order stainless steel, be separated with the deionized water wash laggard row solid-liquid second stage, remove the by-product salt in polyphenylene sulfide product, obtain scavenging solution and wet polyphenylene sulfide product respectively; Wet polyphenylene sulfide product adopt SGZ double-cone vacuum dryer vacuum tightness be-0.05MPa, heating low-pressure steam carries out vacuum-drying under being the condition of 3kg, obtains qualified polyphenylene sulfide resin fat prod after 90 minutes.
embodiment 2produce a method for polyphenylene sulfide washing, purifying, comprise the following steps:
(1) many water cure sodium is dissolved in the solvent NMP(n-methyl-2-pyrrolidone of its quality 3.5 times) in; under the katalysis of auxiliary agent lithium chloride and sheet alkali; the moisture in many water cure sodium is taken off by protection of inert gas; add DCB(santochlor again) and nmp solution; polyreaction is carried out according to a conventional method, synthesis polyphenylene sulfide mixture slip in closed reactor.
Wherein: DCB is 0.85 times of many water cure sodium quality, nmp solution is 1.5 times of many water cure sodium quality.
(2) with sleeping spiral shell sedimentation conveyer centrifugal, polyphenylene sulfide mixture slip is carried out solid-liquid separation, obtain the polyphenylene sulfide resin fat prod containing 5 ~ 10% oligopolymer and the mixture of by-product salt, most of nmp solution respectively.
Wherein: the condition of solid-liquid separation refers to that mixture temperature is 150 DEG C, and centrifugal owner's rotating speed is 3500r/min, and disengaging time is 1.5h.
(3) the mixture of the polyphenylene sulfide resin fat prod containing 5 ~ 10% oligopolymer and by-product salt is joined in leacher, and remove oligopolymer in thick product and most of by-product salt with 4 times of reverse immersions of the deionized water to mixture quality, rinsing, obtain the thick product of polyphenylene sulfide and the rinsing liquid of saliferous respectively.
Wherein: the temperature of deionized water is 95 DEG C.
(4) thick for the polyphenylene sulfide of saliferous product is inputed in the two-in-one strainer of 180 order stainless steel, be separated with the deionized water wash laggard row solid-liquid second stage, remove the by-product salt in polyphenylene sulfide product, obtain scavenging solution and wet polyphenylene sulfide product respectively; Wet polyphenylene sulfide product adopt SGZ double-cone vacuum dryer vacuum tightness be-0.08MPa, heating low-pressure steam carries out vacuum-drying under being the condition of 5kg, obtains qualified polyphenylene sulfide resin fat prod after 110 minutes.
embodiment 3produce a method for polyphenylene sulfide washing, purifying, comprise the following steps:
(1) many water cure sodium is dissolved in the solvent NMP(n-methyl-2-pyrrolidone of its quality 3.0 times) in; under the katalysis of auxiliary agent lithium chloride and sheet alkali; the moisture in many water cure sodium is taken off by protection of inert gas; add DCB(santochlor again) and nmp solution; polyreaction is carried out according to a conventional method, synthesis polyphenylene sulfide mixture slip in closed reactor.
Wherein: DCB is 0.82 times of many water cure sodium quality, nmp solution is 1.2 times of many water cure sodium quality.
(2) with sleeping spiral shell sedimentation conveyer centrifugal, polyphenylene sulfide mixture slip is carried out solid-liquid separation, obtain the polyphenylene sulfide resin fat prod containing 5 ~ 10% oligopolymer and the mixture of by-product salt, most of nmp solution respectively.
Wherein: the condition of solid-liquid separation refers to that mixture temperature is 125 DEG C, and centrifugal owner's rotating speed is 3300r/min, and disengaging time is 1.2h.
(3) the mixture of the polyphenylene sulfide resin fat prod containing 5 ~ 10% oligopolymer and by-product salt is joined in leacher, and remove oligopolymer in thick product and most of by-product salt with 4 times of reverse immersions of the deionized water to mixture quality, rinsing, obtain the thick product of polyphenylene sulfide and the rinsing liquid of saliferous respectively.
Wherein: the temperature of deionized water is 93 DEG C.
(4) thick for the polyphenylene sulfide of saliferous product is inputed in the two-in-one strainer of 180 order stainless steel, be separated with the deionized water wash laggard row solid-liquid second stage, remove the by-product salt in polyphenylene sulfide product, obtain scavenging solution and wet polyphenylene sulfide product respectively; Wet polyphenylene sulfide product adopt SGZ double-cone vacuum dryer vacuum tightness be-0.065MPa, heating low-pressure steam carries out vacuum-drying under being the condition of 4kg, obtains qualified polyphenylene sulfide resin fat prod after 100 minutes.
Claims (4)
1. produce a method for polyphenylene sulfide washing, purifying, comprise the following steps:
(1) many water cure sodium is dissolved in the solvent NMP of its quality 2.5 ~ 3.5 times, under the katalysis of auxiliary agent lithium chloride and sheet alkali, the moisture in described many water cure sodium is taken off by protection of inert gas, add DCB and nmp solution again, polyreaction is carried out according to a conventional method, synthesis polyphenylene sulfide mixture slip in closed reactor; Described DCB is 0.8 ~ 0.85 times of described many water cure sodium quality, and described nmp solution is 1 ~ 1.5 times of described many water cure sodium quality;
(2) with sleeping spiral shell sedimentation conveyer centrifugal, described polyphenylene sulfide mixture slip is carried out solid-liquid separation, obtain the polyphenylene sulfide resin fat prod containing 5 ~ 10% oligopolymer and the mixture of by-product salt, most of nmp solution respectively;
(3) the mixture of described the polyphenylene sulfide resin fat prod and by-product salt that contain 5 ~ 10% oligopolymer is joined in leacher, and remove oligopolymer in thick product and most of by-product salt with 4 times of reverse immersions of the deionized water to mixture quality, rinsing, obtain the thick product of polyphenylene sulfide and the rinsing liquid of saliferous respectively;
(4) thick for the polyphenylene sulfide of described saliferous product is inputed in the two-in-one strainer of 180 order stainless steel, be separated with the deionized water wash laggard row solid-liquid second stage, remove the by-product salt in polyphenylene sulfide product, obtain scavenging solution and wet polyphenylene sulfide product respectively; Described wet polyphenylene sulfide product obtains qualified polyphenylene sulfide resin fat prod through vacuum-drying.
2. as claimed in claim 1 a kind of produce polyphenylene sulfide washing, purifying method, it is characterized in that: described step (2) in the condition of solid-liquid separation refer to that described mixture temperature is 100 ~ 150 DEG C, centrifugal owner's rotating speed is 3000 ~ 3500r/min, and disengaging time is 1 ~ 1.5h.
3. a kind of method of producing polyphenylene sulfide washing, purifying as claimed in claim 1, is characterized in that: described step (3) in the temperature of deionized water be 90 ~ 95 DEG C.
4. as claimed in claim 1 a kind of produce polyphenylene sulfide washing, purifying method, it is characterized in that: described step (4) in vacuum drying condition refer to and adopt SGZ double-cone vacuum dryer, its vacuum tightness is-0.05 ~-0.08MPa, heating low-pressure steam is 3 ~ 5kg, and time of drying is 90 ~ 110 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510298212.7A CN104877135A (en) | 2015-06-04 | 2015-06-04 | Washing and purifying method for polyphenylene sulfide resin production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510298212.7A CN104877135A (en) | 2015-06-04 | 2015-06-04 | Washing and purifying method for polyphenylene sulfide resin production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104877135A true CN104877135A (en) | 2015-09-02 |
Family
ID=53944832
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510298212.7A Pending CN104877135A (en) | 2015-06-04 | 2015-06-04 | Washing and purifying method for polyphenylene sulfide resin production |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104877135A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104817696A (en) * | 2015-03-04 | 2015-08-05 | 常州大学 | Method for desalting purification of polymer product in polyphenylene sulfide production |
| CN105218816A (en) * | 2015-11-05 | 2016-01-06 | 包头市汇智工程咨询有限责任公司 | A kind of resin leaching technology produced for poly arylidene thio-ester resinoid |
| CN105601925A (en) * | 2016-01-19 | 2016-05-25 | 成都汇莹新材料有限公司 | Resin washing technique for production of polyphenylene sulfide |
| CN110527089A (en) * | 2019-07-31 | 2019-12-03 | 长治市霍家工业有限公司 | A kind of purification process producing high-purity polyphenylene sulfide |
| CN110818898A (en) * | 2019-11-22 | 2020-02-21 | 四川轻化工大学 | Method for dehydrating sodium sulfide dihydrate in polyphenylene sulfide production |
| CN111057239A (en) * | 2019-12-28 | 2020-04-24 | 重庆聚狮新材料科技有限公司 | Method for recovering lithium salt auxiliary agent in polyphenylene sulfide production process |
| CN111253573A (en) * | 2019-12-28 | 2020-06-09 | 重庆聚狮新材料科技有限公司 | Method for preparing polyphenylene sulfide resin |
| CN114602876A (en) * | 2022-03-09 | 2022-06-10 | 山东明化新材料有限公司 | High molecular resin washing, separating and purifying method |
| CN115090408A (en) * | 2022-04-28 | 2022-09-23 | 新疆中泰新鑫化工科技股份有限公司 | Polyphenylene sulfide resin washing and purifying device and using method thereof |
| CN116041703A (en) * | 2022-12-30 | 2023-05-02 | 四川大学 | High-whiteness low-impurity-content polyarylether and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102863622A (en) * | 2012-09-25 | 2013-01-09 | 自贡鸿鹤化工股份有限公司 | Method for collecting polyphenylene sulfide resin from polyphenylene sulfide resin slurry |
| CN103694476A (en) * | 2013-12-25 | 2014-04-02 | 济南开发区星火科学技术研究院 | Preparation method of polyphenylene sulfide |
-
2015
- 2015-06-04 CN CN201510298212.7A patent/CN104877135A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102863622A (en) * | 2012-09-25 | 2013-01-09 | 自贡鸿鹤化工股份有限公司 | Method for collecting polyphenylene sulfide resin from polyphenylene sulfide resin slurry |
| CN103694476A (en) * | 2013-12-25 | 2014-04-02 | 济南开发区星火科学技术研究院 | Preparation method of polyphenylene sulfide |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104817696B (en) * | 2015-03-04 | 2018-10-19 | 常州大学 | Polymeric articles desalting purifying method in a kind of production of polyphenylene sulfide |
| CN104817696A (en) * | 2015-03-04 | 2015-08-05 | 常州大学 | Method for desalting purification of polymer product in polyphenylene sulfide production |
| CN105218816A (en) * | 2015-11-05 | 2016-01-06 | 包头市汇智工程咨询有限责任公司 | A kind of resin leaching technology produced for poly arylidene thio-ester resinoid |
| CN105601925A (en) * | 2016-01-19 | 2016-05-25 | 成都汇莹新材料有限公司 | Resin washing technique for production of polyphenylene sulfide |
| CN105601925B (en) * | 2016-01-19 | 2018-01-16 | 成都汇莹新材料有限公司 | A kind of resin washing process technology in polyphenylene sulfide production |
| CN110527089B (en) * | 2019-07-31 | 2022-02-18 | 长治市霍家工业有限公司 | Purification method for producing high-purity polyphenylene sulfide resin |
| CN110527089A (en) * | 2019-07-31 | 2019-12-03 | 长治市霍家工业有限公司 | A kind of purification process producing high-purity polyphenylene sulfide |
| CN110818898A (en) * | 2019-11-22 | 2020-02-21 | 四川轻化工大学 | Method for dehydrating sodium sulfide dihydrate in polyphenylene sulfide production |
| CN110818898B (en) * | 2019-11-22 | 2021-11-19 | 四川轻化工大学 | Method for dehydrating sodium sulfide dihydrate in polyphenylene sulfide production |
| CN111253573A (en) * | 2019-12-28 | 2020-06-09 | 重庆聚狮新材料科技有限公司 | Method for preparing polyphenylene sulfide resin |
| CN111057239A (en) * | 2019-12-28 | 2020-04-24 | 重庆聚狮新材料科技有限公司 | Method for recovering lithium salt auxiliary agent in polyphenylene sulfide production process |
| CN114602876A (en) * | 2022-03-09 | 2022-06-10 | 山东明化新材料有限公司 | High molecular resin washing, separating and purifying method |
| CN115090408A (en) * | 2022-04-28 | 2022-09-23 | 新疆中泰新鑫化工科技股份有限公司 | Polyphenylene sulfide resin washing and purifying device and using method thereof |
| CN115090408B (en) * | 2022-04-28 | 2023-08-22 | 新疆中泰新鑫化工科技股份有限公司 | Polyphenylene sulfide resin washing and purifying device and application method thereof |
| CN116041703A (en) * | 2022-12-30 | 2023-05-02 | 四川大学 | High-whiteness low-impurity-content polyarylether and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104877135A (en) | Washing and purifying method for polyphenylene sulfide resin production | |
| CN102863567B (en) | Preparation method of polyvinyl alcohol through low-alkali method | |
| CN104892971B (en) | Method for recycling solvent NMP in polyphenylene sulfide resin production process | |
| CN104262200B (en) | One recycles waste water and prepares N, N ' production method of-dicyclohexylcarbodiimide | |
| CN102731785B (en) | Polyphenylene sulfide purifying method | |
| CN102634011B (en) | Poly-p-phenylene terephthamide (PPTA) polymer washing and solvent recovery method | |
| CN101570337B (en) | Production method of battery- grade lithium fluoride | |
| CN104877167B (en) | The method that adjuvant used lithium chloride recycles in polyphenylene sulfide resin production process | |
| CN101343232A (en) | Preparation method for 2-chloro-4-nitroaniline | |
| CN111534891B (en) | Polymerization solvent system recovery process in aramid fiber 1414 production | |
| CN110305028B (en) | Device and process for washing glycine crude product by alcohol phase method | |
| CN110527089B (en) | Purification method for producing high-purity polyphenylene sulfide resin | |
| WO2013129405A1 (en) | Method for manufacturing refined methionine | |
| CN102746134A (en) | Method for decreasing content of sodium chloride impurities in recovered sodium formate | |
| CN110105573A (en) | A method of reducing polyphenylene sulfide by-product salt COD | |
| CN106380601A (en) | Purifying method for polyphenylene sulfide with high molecular weight | |
| CN113680128B (en) | Continuous washing and purifying system and purifying method for polyarylene sulfide resin | |
| CN107286345B (en) | Industrial production method of high-purity polysulfone, polyether sulfone and polyarylsulfone resin | |
| CN210656752U (en) | Device for washing glycine crude product by alcohol phase method | |
| CN112778094B (en) | Preparation process of high-purity tetrabromobisphenol A | |
| CN111518861B (en) | Novel process for preparing D-calcium pantothenate | |
| CN110698669B (en) | Method for cleaning poly (p-phenylene terephthalamide) resin | |
| CN108164069B (en) | Treatment method of tetraethylammonium tetrafluoroborate production wastewater | |
| CN106744996A (en) | A kind of Ludox and preparation method thereof | |
| CN103641793A (en) | Treatment method of AE (Active Ester) residual liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150902 |
|
| RJ01 | Rejection of invention patent application after publication |