阅读说明：本技术 一种生产高纯度聚苯硫醚树脂的纯化方法 (A kind of purification process producing high-purity polyphenylene sulfide ) 是由 钟俊敏 董栋芳 霍翔宙 霍伟伟 霍雪芳 苗泽慧 霍冰冰 于 2019-07-31 设计创作，主要内容包括：本发明针对聚苯硫醚树脂纯度不高的问题,公开了一种生产高纯度聚苯硫醚树脂的纯化方法,包括如下步骤：高速离心机内第一次固液分离,加热纯化,高速离心机内第二次固液分离,得到纯化后的树脂半成品；纯化后的树脂半成品破碎,纯水漂洗,漂洗出树脂内的油相杂质；纯水逆流冲洗,除去树脂表面的杂质；纯水浸泡,除去树脂孔隙内的残留杂质；高速离心机内第三次固液分离,干燥,得到高纯度聚苯硫醚树脂成品。本方法能提高聚苯硫醚树脂纯度,得到的树脂杂质少、纯度高,成品树脂灰分低于0.1%,颗粒均匀、大小适中,各项性能更为稳定。(The present invention problem not high for polyphenylene sulfide purity, a kind of purification process for producing high-purity polyphenylene sulfide is disclosed, includes the following steps: to be separated by solid-liquid separation for the first time in supercentrifuge, it is heating purified, it is separated by solid-liquid separation for second in supercentrifuge, obtains resin semi-finished product after purification；Resin semi-finished product after purification are broken, and pure water rinsing rinses out the oily phase impurity in resin；Pure water back flushing removes the impurity of resin surface；Pure water impregnates, and removes the residual impurity in resin voids；Third time is separated by solid-liquid separation in supercentrifuge, dry, obtains high-purity polyphenylene sulfide finished product.This method can improve polyphenylene sulfide purity, and obtained resin impurity is few, with high purity, and sold resin ash content is lower than 0.1%, and particle is uniform, is of moderate size, and properties are more stable.)

1. a kind of purification process for producing high-purity polyphenylene sulfide, which comprises the steps of:

1) it is separated by solid-liquid separation for the first time, the polyphenylene sulfide slurry that polymerization reaction synthesizes is put into isobaric emptying tank, 80- is cooled to 100 degree, 4-6 cubes of speed is put into supercentrifuge material on an hourly basis, is carried out first time separation of solid and liquid, is obtained polyphenylene sulfide Ether semi-finished product resin；

2) it purifies, obtained semi-finished product resin will be separated by solid-liquid separation for the first time and be transferred in purification kettle, solvent NMP is added, unlatching is stirred It mixes, speed of agitator 100-170r/min, is heated to 100-150 degree, kept for temperature in the kettle 100-150 degree 1.5-2.5 hours；

3) it second is separated by solid-liquid separation, 7-9 cubes of speed is put into supercentrifuge to resin and refined solution after purification on an hourly basis It is interior, it carries out second and is separated by solid-liquid separation, obtain resin semi-finished product after purification；

4) it is crushed, resin semi-finished product after purification are put to crusher, and the partial size and particle of broken material to 50-60 microns are uniform Solid resin beads；

5) it rinses, broken resin is put to subsider, and pure water is added, and is carried out sedimentation washing, wash time 2-4 hours, is floated Wash out the oily phase impurity in resin；

6) it rinses, the resin after the completion of rinsing is put into desalinization of soil by flooding or leaching machine, and by the water velocity of 4-6m3/h, pure water back flushing is added 3-5 hours, remove the impurity of resin surface；

7) it impregnates, resin is sent to semi-finished product material stock tank after the completion of flushing, and pure water is added and impregnates 3-5 hours, removes resin voids Interior residual impurity；

8) third time is separated by solid-liquid separation, and the semi-finished product slurry after the completion of impregnating, 4-5 cubes of speed is put into high speed centrifugation on an hourly basis In machine, third time separation of solid and liquid is carried out, the polyphenylene sulfide semi-finished product of high-purity are obtained；

9) dry, the polyphenylene sulfide semi-finished product of obtained high-purity will be separated by solid-liquid separation for the third time, be put in drying machine, carried out It is dry, obtain high-purity polyphenylene sulfide finished product.

2. a kind of purification process for producing high-purity polyphenylene sulfide according to claim 1, which is characterized in that described The mass ratio of NMP and solid material is NMP: solid material=1:0.5-2 in step 2.

3. a kind of purification process for producing high-purity polyphenylene sulfide according to claim 1, which is characterized in that described The mass ratio of pure water and solid material is pure water: solid material=1:3-4 in step 5).

4. a kind of purification process for producing high-purity polyphenylene sulfide according to claim 1, which is characterized in that described The impurity of resin surface includes but is not limited to chloride and catalyst residual in step 6).

5. a kind of purification process for producing high-purity polyphenylene sulfide according to claim 1, which is characterized in that described In step 6) whether the completion of flushing process, judged by carrying out conductivity monitoring to the washing water after pure water rinsing.

6. a kind of purification process for producing high-purity polyphenylene sulfide according to claim 1, which is characterized in that described The mass ratio of pure water and resin is pure water: resin=1:3-8 in step 7).

7. a kind of purification process for producing high-purity polyphenylene sulfide according to claim 1, which is characterized in that described The polyphenylene sulfide semi-finished product of obtained high-purity are separated by solid-liquid separation for the third time, also by successively carrying out: secondarily purified, the 4th Secondary separation of solid and liquid, secondary rinsing, secondary flushing, secondary immersion and the 5th separation of solid and liquid, drying, obtain high-purity polyphenylene sulfide Resin finished product.

8. a kind of purification process for producing high-purity polyphenylene sulfide according to claim 7, which is characterized in that described Secondarily purified condition are as follows: in purification kettle, solvent sulfolane is added, the dosage of the sulfolane is the polyphenylene sulfide of high-purity 3-10 times of semi-finished product, secondarily purified to carry out under stirring, the speed of agitator is 150r/min, is heated to 130-150 Degree is kept for temperature in the kettle 130-150 degree 2-5 hours, dissolves and be adhered to a small amount of ash content on resin.

Technical field

A kind of purification process for producing high-purity polyphenylene sulfide of the present invention, belongs to polyphenylene sulfide production technical field.

Background technique

The enterprise of domestic production polyphenylene sulfide at present, molecular weight, hot property, the mechanical property of polyphenylene sulfide produced The indexs such as energy, it is very nearly the same compared with the U.S., Japan's polyphenylene sulfide produced.But in terms of the purity of resin, domestic institute The problem that the generally existing purity of the resin of production is not high, impurity is on the high side, impurity are mostly chloride, catalyst residual, polymerization mother Liquid residual, incomplete polymer etc..Resin purity is not high will affect down-stream enterprise using resin injection moulding, fibre spinning at The problems such as product yield is low, mechanical property is bad, product quality is unqualified.

Aiming at the problem that polyphenylene sulfide resin purifying, domestic enterprise is generally removed using the mode of water flow flushing, filtering The impurity of resin can not thoroughly solve the problems, such as that resin purity is not high, resin finished product is still because of the limitation of its operational characteristic The problems such as it is higher that there are impurity, and resin whiteness is inadequate, to downstream, resin processing enterprise brings puzzlement.

Summary of the invention

To solve the shortcomings of the prior art, the present invention problem not high for polyphenylene sulfide purity is disclosed A kind of purification process producing high-purity polyphenylene sulfide, can improve polyphenylene sulfide purity, obtained resin impurity is few, Purity is high, particle is uniform, is of moderate size, and properties are more stable.

The invention is realized by the following technical scheme:

A kind of purification process producing high-purity polyphenylene sulfide, includes the following steps:

1) it is separated by solid-liquid separation for the first time, the polyphenylene sulfide slurry that polymerization reaction synthesizes is put into isobaric emptying tank, 80- is cooled to 100 degree, 4-6 cubes of speed is put into supercentrifuge material on an hourly basis, is carried out first time separation of solid and liquid, is obtained polyphenylene sulfide Ether semi-finished product resin；Material can reach better separating effect using the speed.

2) it purifies, obtained semi-finished product resin will be separated by solid-liquid separation for the first time and be transferred in purification kettle, solvent NMP is added, opens Stirring is opened, speed of agitator 100-170r/min is heated to 100-150 degree, keeps temperature in the kettle 100-150 degree 1.5-2.5 small When；

3) it second is separated by solid-liquid separation, 7-9 cubes of speed is put into supercentrifuge to resin and refined solution after purification on an hourly basis It is interior, it carries out second and is separated by solid-liquid separation, obtain resin semi-finished product after purification；

4) it is crushed, resin semi-finished product after purification are put to crusher, and the partial size and particle of broken material to 50-60 microns are uniform Solid resin beads；

5) it rinses, broken resin is put to subsider, and pure water is added, and is carried out sedimentation washing, wash time 2-4 hours, is floated Wash out the oily phase impurity in resin；

6) it rinses, the resin after the completion of rinsing is put into desalinization of soil by flooding or leaching machine, and by the water velocity of 4-6m3/h, pure water back flushing is added 3-5 hours, remove the impurity of resin surface；The impurity of the resin surface includes but is not limited to that chloride and catalyst are residual It stays.Whether the completion of the rinsing step, judged by carrying out conductivity monitoring to the washing water after pure water rinsing.

In order to preferably wash the salinity of resin, because having salinity in resin, and polyphenylene sulfide institute salt concentration is in water Middle 10-15% just reaches saturation, so for the better desalinization of soil by flooding or leaching and impurity, the water velocity 4-6m3/h that provides.Material is up It walks, water is toward undershoot, the great efforts of flushing, and washing effect is good.

7) it impregnates, resin is sent to semi-finished product material stock tank after the completion of flushing, and pure water is added, and is impregnated 3-5 hours, and resin is removed Intrapore residual impurity；

8) third time is separated by solid-liquid separation, and the semi-finished product slurry after the completion of impregnating, 4-5 cubes of speed is put into high speed centrifugation on an hourly basis In machine, third time separation of solid and liquid is carried out, the polyphenylene sulfide semi-finished product of high-purity are obtained；

9) dry, the polyphenylene sulfide semi-finished product of obtained high-purity will be separated by solid-liquid separation for the third time, be put in drying machine, carried out It is dry, obtain high-purity polyphenylene sulfide finished product.

The mass ratio of NMP and solid material is NMP: solid material=1:3-4 in the step 2.

The mass ratio of pure water and solid material is pure water: solid material=1:3-4 in the step 5).

The mass ratio of pure water and resin is pure water: resin=1:3-8 in the step 7).

Preferably, the polyphenylene sulfide semi-finished product for the high-purity that the third time is separated by solid-liquid separation, also by successively Carry out: secondarily purified, the 4th separation of solid and liquid, secondary rinsing, secondary flushing, secondary immersion are separated by solid-liquid separation with the 5th time, are dry It is dry, obtain high-purity polyphenylene sulfide finished product.

The secondarily purified condition are as follows: in purification kettle, solvent sulfolane is added, the dosage of the sulfolane is high-purity 3-10 times of polyphenylene sulfide semi-finished product, secondarily purified to carry out under stirring, the speed of agitator is 150r/min, is added Heat is kept for temperature in the kettle 130-150 degree 2-5 hours to 130-150 degree, dissolves and be adhered to a small amount of ash content on resin.

Sulfolane low toxicity is inexpensive, can adsorb the ash content in resin, effectively purification resin, obtains the polyphenylene sulfide resin of high whiteness Rouge.

4th separation of solid and liquid, it is secondarily purified after resin and refined solution 4-6 cubes of speed is put on an hourly basis In supercentrifuge, carries out second and be separated by solid-liquid separation；

The secondary rinsing, the 4th time be separated by solid-liquid separation after resin put to subsider, be added pure water, carry out sedimentation washing, institute The mass ratio for stating pure water and solid material is pure water: solid material=1:2-4 wash time 1-2 hours, rinses out in resin Oily phase impurity；

The secondary flushing, the resin after the completion of secondary rinsing, is put into desalinization of soil by flooding or leaching machine, pure water is added, by the water flow velocity of 2-4m3/h Degree back flushing 1-2 hours removes the impurity such as chloride and the catalyst residual of resin surface；The completion of secondary flushing with It is no, judged by carrying out conductivity monitoring to the washing water after pure water rinsing, when the conductivity of washing water is lower than 20S/m, Judgement washing is completed；

The secondary immersion, resin is sent to semi-finished product material stock tank after the completion of secondary flushing, and it is small that pure water 4-6m3 immersion 1-3 is added When, remove the residual impurity in resin voids；

5th separation of solid and liquid, the semi-finished product slurry after the completion of secondary immersion, 1-3 cubes of speed is put into height on an hourly basis In fast centrifuge, the 5th separation of solid and liquid is carried out；

Compared with the prior art, the invention has the following beneficial effects:

This method can effectively improve the purity of polyphenylene sulfide, sedimentation is washed by sedimentation washing, back flushing and washing by soaking It washs, rinses out the oily phase impurity in resin, pure water back flushing removes the impurity of resin surface；Pure water impregnates, and removes resin hole Residual impurity in gap.It can be effectively to the various impurity in outer removing resin by these three steps.

The method of the present invention is simple, and equipment cost is low, and in the prior art, some methods are needed using ultrasonic equipment, ultrasound Wave device is at high price, and production investment is very big.

Resin impurity made from method of the invention is few, with high purity, and sold resin ash content is lower than 0.1%, makes the items of resin Performance is more stable.

Resin chloride content hereinafter, reach food-grade raw material requirement, has expanded the application range of resin in 50 PPM.

Because polymer content incomplete in its resin is lower than 0.2%, so that resin be made to answer in injection molding, fiber draw In, possess more excellent mechanical property.

Resin particle is uniform, is of moderate size, and also brings convenience using enterprise for downstream, reduces resin in post-processing Loss in journey.

The resin of high-purity, the impurity on strand end group is few, thus the phenomenon that being avoided that resin jaundice, end group oxidation, Resin is set to possess excellent antioxygenic property.Because of its purity is high, the whiteness of resin is made to be held at 90Wr or more.

Specific embodiment

The present invention is described in further detail combined with specific embodiments below, but protection scope of the present invention is not Be limited to these embodiments, it is all without departing substantially from the change of present inventive concept or equivalent substitute be included in protection scope of the present invention it It is interior.