CN104277220A - Method for removing salts out of polyphenyl thioether recovery solvent - Google Patents
Method for removing salts out of polyphenyl thioether recovery solvent Download PDFInfo
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Abstract
The invention relates to a method for removing salts out of a polyphenyl thioether recovery solvent. The method comprises the following steps of: after sodium sulfide method polyphenyl thioether synthesis reaction is finished, cooling slurry, filtering, washing a polyphenyl thioether filter cake by using low-boiling -point alcohol, and displacing an N-methyl pyrrolidone solvent contained in the polyphenyl thioether filter cake; after the reaction between alcohol washing liquor and polyphenyl thioether is finished, mixing with the filtrate obtained by cooling and filtering the slurry, rectifying at normal pressure to remove the low-boiling point alcohol, and then carrying out reduced pressure distillation to recover the N-methyl pyrrolidone solvent; washing the filter cake which contains sodium chloride, the low-boiling point alcohol and polyphenyl thioether by using desalted water, centrifugally separating, rectifying centrifugate at normal pressure to recover the low-boiling point alcohol, and discharging or evaporating salt-containing water to obtain solid sodium chloride. According to the method, no dehydration process is carried out in a solvent recovery process, so that the phenomena of precipitation and stacking of salt crystals are prevented; when the low-boiling point alcohol is recovered, no water or only a small amount of water is evaporated, and salt is dissolved in water inside a tower kettle without crystal precipitation and can be discharged or further evaporated so as to obtain a by-product sodium chloride.
Description
Technical field
The present invention relates to solvent recuperation technology, particularly a kind of method removing salt in polyphenylene sulfide recycling design.
Background technology
Sodium sulfide method is one of prevailing technology of polyphenylene sulfide synthesis, and N-Methyl pyrrolidone (NMP) synthesizes the most frequently used organic solvent of polyphenylene sulfide.In sodium sulfide method synthesis polyphenylene sulfide process, often produce one ton of polyphenylene sulfide and can generate 1.08 tons of sodium-chlor.N-Methyl pyrrolidone solvent price is higher, and emission request is strict, all needs to reclaim N-Methyl pyrrolidone solvent from environmental protection or cost angle as far as possible.Domestic polyphenylene sulfide actual output is far smaller than its production capacity, and one of its reason is that the rate of recovery is low, and easily causes the phenomenons such as process pipe blocking in removal process because the existence of a large amount of salt makes solvent recuperation cost high.
Domestic many producers polyphenylene sulfide solvent recuperation adopts following technique, shown in Fig. 2: polyphenylene sulfide building-up reactions terminates disposed slurry cooling and filters, filter cake is washed, water lotion mixes rectification under vacuum and dewaters with filtrate, wherein mixed solution composition N-Methyl pyrrolidone (NMP) accounts for 45%, water accounts for 45%, salt and other account for 10%.After rectifying and dewatering, mixed solution carries out sedimentation, and N-Methyl pyrrolidone (NMP) is reclaimed in supernatant liquid rectification under vacuum; Settled slurry is centrifugal, and N-Methyl pyrrolidone (NMP) is reclaimed in centrifugate rectification under vacuum; Filter cake drying under reduced pressure, in drying process, N-Methyl pyrrolidone (NMP) is reclaimed in phlegma rectification under vacuum.This processing disadvantages removes sodium-chlor crystallization in rectifying tower reactor when rectification under vacuum is dewatered along with water, is deposited in tower reactor and affects heating efficiency, and be difficult to sodium-chlor emptying during blowing; Although salt-cake drying under reduced pressure can reclaim N-Methyl pyrrolidone (NMP), dust blocking filtering net and the pipeline accident of salt easily occurs, cause solvent recuperation in salt to interrupt, or solvent recuperation is incomplete, the total rate of recovery of solvent is low.
Summary of the invention
Technical problem to be solved by this invention, by removing the salt in sodium sulfide method synthesis polyphenylene sulfide recycling design, being avoided salt to pile up at solvent recovery tower tower reactor intercrystalline, also being carried out drying without solvent-laden salt-cake, further recycling design.Concrete technical scheme of the present invention is as follows:
The method of salt in removal polyphenylene sulfide recycling design of the present invention, slurry polyphenylene sulfide building-up reactions terminated cooling is filtered; With low-boiling point alcohol washing polyphenylene sulfide filter cake, N-Methyl pyrrolidone solvent in displacement filter cake, alcohol washing lotion and polyphenylene sulfide react and terminate the disposed slurry filtrate of filtering of lowering the temperature and mix, and to remove after low-boiling point alcohol rectification under vacuum again reclaim N-Methyl pyrrolidone solvent through atmospheric distillation; The de-salted water washing of the filter cake of sodium chloride-containing, low-boiling point alcohol, polyphenylene sulfide, centrifugation, centrifugate atmospheric distillation reclaims low-boiling point alcohol, and tower reactor is that brackish water is arranged outward or evaporated and obtains solid sodium chloride.
Concrete steps are as follows:
Remove a method for salt in polyphenylene sulfide recycling design, it is characterized in that method is as follows:
1) the slurry cooling of the polyphenylene sulfide generated for raw material reaction with sodium sulphite, santochlor is filtered;
2) step 1) polyphenylene sulfide filter cake low-boiling point alcohol wash, displacement filter cake in N-Methyl pyrrolidone solvent, alcohol washing lotion and step 1) filtration after filtrate mix;
3) step 2) with step 1) mixed filtrate to remove after low-boiling point alcohol rectification under vacuum again through atmospheric distillation and reclaims N-Methyl pyrrolidone solvent;
4) step 2) filter cake de-salted water washing, centrifugation after alcohol wash, centrifugate atmospheric distillation reclaims low-boiling point alcohol, and brackish water is arranged outward or evaporated and obtains solid sodium chloride.
Described step 2) low-boiling point alcohol refers to the methyl alcohol or ethanol etc. of boiling point lower than water boiling point, water Han Liang≤5% in alcohol.
Described step 2) polyphenylene sulfide filter cake low-boiling point alcohol washing be that cover is washed or washed successively by lower boiling fresh alcohol.
Described alcohol washes N-Methyl pyrrolidone solvent in polyphenylene sulfide filter cake can wash displacement successively with fresh methanol, ethanol, also can wash displacement with cover; Fresh methanol, washing with alcohol polyphenylene sulfide filter cake number of times 3 ~ 4 times, cover washes polyphenylene sulfide filter cake number of times 4 ~ 5 times.
Described methyl alcohol or washing with alcohol polyphenylene sulfide filter cake pressure are normal pressure, and wash temperature is normal temperature ~ methyl alcohol or ethanol atmospheric boiling point temperature; Methyl alcohol or ethanol consumption are 400 ~ 500ml/100g polyphenylene sulfide filter cake.
Described step 4) filter cake de-salted water is washed after alcohol wash, and de-salted water washing can be the washing of fresh de-salted water, and washing times is 3 ~ 4 times; Also can be that cover washes with water, number of times washed by cover be 4 ~ 5 times; De-salted water washing pressure is normal pressure, and washing temperature is carried out under 60 DEG C ~ reflux temperature; The consumption of de-salted water is 300 ~ 400ml/100g polyphenylene sulfide filter cake.
Described alcohol wash or washing are under agitation carried out.
Described step 3) lower boiling fresh alcohol successively washings and polyphenylene sulfide reacted and terminate the disposed slurry filtrate of filtering of lowering the temperature and mix, atmospheric distillation after taking off low-boiling point alcohol again rectification under vacuum reclaim N-Methyl pyrrolidone; First time cover is washed low-boiling point alcohol washing lotion and polyphenylene sulfide to react and terminate the disposed slurry filtrate of filtering of lowering the temperature and mix, atmospheric distillation to take off after low-boiling point alcohol rectification under vacuum recovery N-Methyl pyrrolidone again.
Described step 4) centrifugate atmospheric distillation recovery low-boiling point alcohol, after referring to fresh de-salted water repeatedly to be washed centrifugate mixing, atmospheric distillation reclaims methyl alcohol or ethanol, obtains the methyl alcohol of Han Liang≤95% or the ethanol of Han Liang≤95%; Or desalination water jacket washes first time washing centrifugate atmospheric distillation recovery methyl alcohol or ethanol, obtain containing the methyl alcohol of amount≤95% or the ethanol containing amount≤95%.
The present invention utilizes low-boiling point alcohol and N-Methyl pyrrolidone (NMP) to dissolve each other, and sodium-chlor and polyphenylene sulfide recycling design separate by the sodium-chlor character that solubleness is low in low-boiling point alcohol, N-Methyl pyrrolidone; Utilize the boiling point of low-boiling point alcohol lower than the physical property of the boiling point of water, reclaim low-boiling point alcohol by atmospheric distillation and do not need to remove water, sodium-chlor is dissolved in tower reactor water, avoids salt-pepper noise in solvent recovery process and separates out.The present invention compared with prior art N-methyl pyrrolidone-free (NMP) solvent recuperation time rectifying and dewatering process, avoid sodium-chlor crystallization, packing phenomenon in rectifying tower reactor; When reclaiming low-boiling point alcohol, do not steam or only steam a small amount of water, salt nodeless mesh is separated out, and is dissolved in tower reactor water, can arrange in addition or further evaporation process, obtain side product chlorinated sodium.
Accompanying drawing explanation
Fig. 1: remove salt FB(flow block) in sodium sulfide method polyphenylene sulfide recycling design.
Fig. 2: domestic many producers polyphenylene sulfide solvent recuperation FB(flow block).
Embodiment
Below by specific embodiment, the invention will be further described.Step is as shown in Figure 1:
1) the slurry cooling of the polyphenylene sulfide generated for raw material reaction with sodium sulphite, santochlor is filtered;
2) step 1) polyphenylene sulfide filter cake low-boiling point alcohol wash, displacement filter cake in N-Methyl pyrrolidone solvent, alcohol washing lotion and step 1) filtration after filtrate mix;
3) step 2) with step 1) mixed filtrate to remove after low-boiling point alcohol rectification under vacuum again through atmospheric distillation and reclaims N-Methyl pyrrolidone solvent;
4) step 2) filter cake de-salted water washing, centrifugation after alcohol wash, centrifugate atmospheric distillation reclaims low-boiling point alcohol, and brackish water is arranged outward or evaporated and obtains solid sodium chloride.
Embodiment 1
Polyphenylene sulfide building-up reactions terminates disposed slurry cooling and filters, under normal temperature and pressure stirs, polyphenylene sulfide filter cake is washed with anhydrous methanol, 100g filter cake anhydrous methanol 400ml, washing time 30 minutes, centrifuging, filter cake washs by above-mentioned condition again, and wash 4 times altogether, the 4th alcohol washing lotion can't detect N-Methyl pyrrolidone.4 alcohol washing lotions are mixed methanol removal, then rectification under vacuum recycling design N-Methyl pyrrolidone (NMP) at pressure 10kpaA, temperature 127 DEG C at atmospheric distillation temperature 64 DEG C with reaction paste filtrate, the salt-free crystallization of cauldron bottom residue.
Embodiment 2
Polyphenylene sulfide building-up reactions terminates disposed slurry cooling and filters, methyl alcohol boiling point 64 DEG C is heated to content 95% methyl alcohol, atmospheric pressure reflux stirs lower washing polyphenylene sulfide filter cake, 100g filter cake methyl alcohol 500ml, washing time 30 minutes, centrifuging, filter cake washs by above-mentioned condition again, wash 3 times altogether, the 3rd time alcohol washing lotion can't detect N-Methyl pyrrolidone.3 alcohol washing lotions are mixed methanol removal at atmospheric distillation temperature 64 DEG C with reaction paste filtrate, rectification under vacuum recycling design N-Methyl pyrrolidone (NMP) at pressure 10kpaA, temperature 127 DEG C, the salt-free crystallization of cauldron bottom residue.
Embodiment 3
Polyphenylene sulfide building-up reactions terminates disposed slurry cooling and filters, and applies mechanically washing polyphenylene sulfide filter cake, 100g filter cake ethanol 500ml, washing time 30 minutes, centrifuging with content 95% ethanol under heating 70 DEG C of atmospheric agitation.It is second time alcohol washing lotion last time that first time applies mechanically washing ethanol, it is third time last time alcohol washing lotion that second time applies mechanically washing ethanol, it is upper order four alcohol washing lotions that third time applies mechanically washing ethanol, 4th time is applied mechanically washing ethanol is fresh 95% ethanol, wash 4 times altogether, the 4th alcohol washing lotion can't detect N-Methyl pyrrolidone.Ethanol is removed, rectification under vacuum recycling design N-Methyl pyrrolidone (NMP) at pressure 10kpaA, temperature 127 DEG C, the salt-free crystallization of cauldron bottom residue 1st alcohol washing lotion is mixed atmospheric distillation temperature 78 DEG C with reaction paste filtrate at.
Embodiment 4
Polyphenylene sulfide building-up reactions terminates disposed slurry cooling and filters, and is being heated to ethyl alcohol boiling point 78 DEG C with dehydrated alcohol, applies mechanically washing polyphenylene sulfide filter cake, 100g filter cake ethanol 400ml, washing time 30 minutes, centrifuging under backflow atmospheric agitation.It is second time alcohol washing lotion last time that first time applies mechanically washing ethanol, it is third time last time alcohol washing lotion that second time applies mechanically washing ethanol, it is upper order four alcohol washing lotions that third time applies mechanically washing ethanol, applying mechanically washing ethanol for 4th time is upper order five alcohol washing lotions, 5th time is applied mechanically washing ethanol is fresh dehydrated alcohol, wash 5 times altogether, the 5th alcohol washing lotion can't detect N-Methyl pyrrolidone.Ethanol is removed, rectification under vacuum recycling design N-Methyl pyrrolidone (NMP) at pressure 10kpaA, temperature 127 DEG C, cauldron bottom residue salt-free crystallization first time alcohol washing lotion to be mixed atmospheric distillation temperature 78 DEG C with reaction paste filtrate at.
Embodiment 5
Polyphenylene sulfide filter cake de-salted water agitator treating after methanol wash, 100g filter cake de-salted water 300ml, be heated to backflow washing, washing time 30 minutes, centrifuging, filter cake is washed by above-mentioned condition again, wash 4 times altogether, by 4 water lotion mixing, atmospheric distillation methanol removal at 64 DEG C, obtain content more than 95% methyl alcohol, saliferous 2.5% in water.
Embodiment 6
The fresh de-salted water agitator treating of polyphenylene sulfide filter cake after methanol wash, the fresh de-salted water 300ml of 100g filter cake, washing temperature 60 DEG C, washing time 30 minutes, centrifuging, filter cake is washed by above-mentioned condition again, washs 4 times altogether, by 4 water lotion mixing, atmospheric distillation methanol removal at 64 DEG C.Obtain content more than 95% methyl alcohol, saliferous 2.5% in tower reactor water.
Embodiment 7
The fresh de-salted water agitator treating of polyphenylene sulfide filter cake after washing with alcohol, the fresh de-salted water 400ml of 100g filter cake, washing temperature 70 DEG C, washing time 30 minutes, centrifuging, filter cake is washed by above-mentioned condition again, washs 3 times altogether, 3 water lotion mixing, at 78 DEG C, atmospheric distillation removes ethanol.Obtain content more than 95% ethanol, saliferous 2.3% in tower reactor water.
Embodiment 8
Polyphenylene sulfide filter cake de-salted water after washing with alcohol is heated to backflow atmospheric agitation and traps washing, 100g filter cake de-salted water 400ml, washing time 30 minutes, centrifuging.First time, cover scouring water was overlapped for the second time last time to wash centrifugate, and second time cover scouring water is overlapped third time last time to wash centrifugate, and cover scouring water is that centrifugate washed by upper order four covers for the third time, and the 4th time cover scouring water is fresh de-salted water, washes 4 times altogether.First time water lotion atmospheric distillation at 78 DEG C is removed ethanol, obtains content more than 95% ethanol, in tower reactor, water evaporation obtains solid salt, and process 100g filter cake obtains 25g solid salt.
Embodiment 9
Polyphenylene sulfide filter cake de-salted water after methanol wash is heated to backflow atmospheric agitation and traps washing, 100g filter cake de-salted water 300ml, washing time 30 minutes, centrifuging.It is overlapped for the second time last time to wash centrifugate that first time overlaps scouring water, second time cover scouring water is overlapped third time last time to wash centrifugate, it is that centrifugate washed by upper order four covers that third time overlaps scouring water, 4th time cover scouring water is that centrifugate washed by upper order five covers, and the 5th time cover scouring water is fresh de-salted water, washes 5 times altogether, first time water lotion atmospheric distillation methanol removal at 64 DEG C, obtain content more than 95% methyl alcohol, in tower reactor, water evaporation obtains solid salt, and process 100g filter cake obtains 25g solid salt.
Claims (9)
1. remove a method for salt in polyphenylene sulfide recycling design, it is characterized in that method is as follows:
1) the slurry cooling of the polyphenylene sulfide generated for raw material reaction with sodium sulphite, santochlor is filtered;
2) step 1) polyphenylene sulfide filter cake low-boiling point alcohol wash, displacement filter cake in N-Methyl pyrrolidone solvent, alcohol washing lotion and step 1) filtration after filtrate mix;
3) step 2) with step 1) mixed filtrate to remove after low-boiling point alcohol rectification under vacuum again through atmospheric distillation and reclaims N-Methyl pyrrolidone solvent;
4) step 2) filter cake de-salted water washing, centrifugation after alcohol wash, centrifugate atmospheric distillation reclaims low-boiling point alcohol, and brackish water is arranged outward or evaporated and obtains solid sodium chloride.
2. the method for claim 1, is characterized in that described step 2) low-boiling point alcohol refers to that boiling point is lower than the methyl alcohol of water boiling point or ethanol, water Han Liang≤5% in alcohol.
3. the method for claim 1, is characterized in that described step 2) polyphenylene sulfide filter cake low-boiling point alcohol washing be that cover is washed or washed successively by lower boiling fresh alcohol.
4. the method as described in claim 1,3, it is characterized in that described polyphenylene sulfide filter cake low-boiling point alcohol washs, fresh low-boiling point alcohol washs polyphenylene sulfide filter cake number of times 3 ~ 4 times successively; The polyphenylene sulfide filter cake number of times adopting cover to wash 4 ~ 5 times.
5. the method for claim 1, it is characterized in that described methyl alcohol or washing with alcohol polyphenylene sulfide filter cake pressure are normal pressure, wash temperature is the atmospheric boiling point temperature of normal temperature ~ low-boiling point alcohol; Methyl alcohol or ethanol consumption are 400 ~ 500ml/100g polyphenylene sulfide filter cake.
6. the method for claim 1, is characterized in that described step 4) filter cake de-salted water is washed after alcohol wash, and de-salted water washing is washed with fresh de-salted water, and washing times is 3 ~ 4 times; Wash with water with cover, number of times washed by cover is 4 ~ 5 times; De-salted water washing pressure is normal pressure, and temperature is carried out under 60 DEG C ~ reflux temperature; The consumption of de-salted water is 300 ~ 400ml/100g polyphenylene sulfide filter cake.
7. the method for claim 1, is characterized in that described alcohol wash or washing are under agitation carried out.
8. method according to claim 1, it is characterized in that described step 3) lower boiling fresh alcohol successively washings and polyphenylene sulfide are reacted and terminate the disposed slurry filtrate of filtering of lowering the temperature and mix, atmospheric distillation after taking off low-boiling point alcohol again rectification under vacuum reclaim N-Methyl pyrrolidone; First time cover is washed low-boiling point alcohol washing lotion and polyphenylene sulfide to react and terminate the disposed slurry filtrate of filtering of lowering the temperature and mix, atmospheric distillation to take off after low-boiling point alcohol rectification under vacuum recovery N-Methyl pyrrolidone again.
9. method according to claim 1, it is characterized in that described step 4) centrifugate atmospheric distillation recovery low-boiling point alcohol, after referring to fresh de-salted water repeatedly to be washed centrifugate mixing, atmospheric distillation reclaims methyl alcohol or ethanol, obtains the methyl alcohol of Han Liang≤95% or the ethanol of Han Liang≤95%; Or desalination water jacket washes first time washing centrifugate atmospheric distillation recovery methyl alcohol or ethanol, obtain containing the methyl alcohol of amount≤95% or the ethanol containing amount≤95%.
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Cited By (9)
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| CN105439935A (en) * | 2015-11-05 | 2016-03-30 | 包头市汇智工程咨询有限责任公司 | Separation process for recovering light components from polyarylene sulfide resin production solvent |
| CN106478481A (en) * | 2016-10-08 | 2017-03-08 | 南京大学 | Waste water ultra-pure separation and purification technique of methyl pyrrolidone containing N and paracide |
| CN106565581A (en) * | 2016-10-21 | 2017-04-19 | 天津科技大学 | A method for comprehensive recovery and utilization of lithium containing mixed salts in a polyphenylene sulfide production process |
| CN107936288A (en) * | 2017-11-30 | 2018-04-20 | 珠海长先新材料科技股份有限公司 | A kind of method of NMP and LiCl in the recycling polyphenylene sulfide production by solvent extraction process technology |
| CN110105573A (en) * | 2019-05-21 | 2019-08-09 | 中国石油化工股份有限公司 | A method of reducing polyphenylene sulfide by-product salt COD |
| CN112552528A (en) * | 2020-11-19 | 2021-03-26 | 万华化学集团股份有限公司 | Method for removing solvent in high-temperature-resistant polymer solution |
| CN112940255A (en) * | 2021-04-14 | 2021-06-11 | 深圳市华盈新材料有限公司 | Purification treatment process of polyphenylene sulfide resin |
| CN113680128A (en) * | 2021-07-27 | 2021-11-23 | 山东明化新材料有限公司 | Continuous washing and purifying system and purifying method for polyarylene sulfide resin |
| CN117756692A (en) * | 2023-12-14 | 2024-03-26 | 四川熔增环保科技有限公司 | Recovery method of N-methyl pyrrolidone |
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| CN105439935A (en) * | 2015-11-05 | 2016-03-30 | 包头市汇智工程咨询有限责任公司 | Separation process for recovering light components from polyarylene sulfide resin production solvent |
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| CN106478481B (en) * | 2016-10-08 | 2018-07-06 | 南京大学 | The ultra-pure separation and purification technique of waste water containing N-Methyl pyrrolidone and paracide |
| CN106565581A (en) * | 2016-10-21 | 2017-04-19 | 天津科技大学 | A method for comprehensive recovery and utilization of lithium containing mixed salts in a polyphenylene sulfide production process |
| CN106565581B (en) * | 2016-10-21 | 2019-07-12 | 天津科技大学 | The comprehensive reutilization method of mixed salt containing lithium in a kind of polyphenylene sulfide production process |
| CN107936288A (en) * | 2017-11-30 | 2018-04-20 | 珠海长先新材料科技股份有限公司 | A kind of method of NMP and LiCl in the recycling polyphenylene sulfide production by solvent extraction process technology |
| CN110105573A (en) * | 2019-05-21 | 2019-08-09 | 中国石油化工股份有限公司 | A method of reducing polyphenylene sulfide by-product salt COD |
| CN110105573B (en) * | 2019-05-21 | 2022-03-08 | 中国石油化工股份有限公司 | Method for reducing COD (chemical oxygen demand) of polyphenylene sulfide byproduct salt |
| CN112552528A (en) * | 2020-11-19 | 2021-03-26 | 万华化学集团股份有限公司 | Method for removing solvent in high-temperature-resistant polymer solution |
| CN112940255A (en) * | 2021-04-14 | 2021-06-11 | 深圳市华盈新材料有限公司 | Purification treatment process of polyphenylene sulfide resin |
| CN112940255B (en) * | 2021-04-14 | 2023-02-17 | 深圳市华盈新材料有限公司 | Purification treatment process of polyphenylene sulfide resin |
| CN113680128A (en) * | 2021-07-27 | 2021-11-23 | 山东明化新材料有限公司 | Continuous washing and purifying system and purifying method for polyarylene sulfide resin |
| CN117756692A (en) * | 2023-12-14 | 2024-03-26 | 四川熔增环保科技有限公司 | Recovery method of N-methyl pyrrolidone |
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