CN102617323A - Method for recovering pentaerythritol and sodium formate - Google Patents
Method for recovering pentaerythritol and sodium formate Download PDFInfo
- Publication number
- CN102617323A CN102617323A CN2012100547921A CN201210054792A CN102617323A CN 102617323 A CN102617323 A CN 102617323A CN 2012100547921 A CN2012100547921 A CN 2012100547921A CN 201210054792 A CN201210054792 A CN 201210054792A CN 102617323 A CN102617323 A CN 102617323A
- Authority
- CN
- China
- Prior art keywords
- sodium formiate
- tetramethylolmethane
- sodium formate
- obtains
- solution
- 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
Images
Abstract
The invention discloses a method for recovering pentaerythritol and sodium formate. Sodium formate coarse materials and sodium formate mother liquid are obtained through evaporating and centrifuging pentaerythritol mother liquid; the obtained sodium formate coarse materials are fed into a drier to be dried to obtain sodium formate with the content being 93 percent; meanwhile, the obtained sodium formate mother liquid accounting for 60 percent of the total weight and the obtained sodium formate with the content being 93 percent are conveyed to a dissolution tank, in addition, water is added, and then, the mixed liquid is stirred for sufficient dissolution; then, the obtained mixed liquid is fed into a centrifugation machine to be centrifuged again, and pentaerythritol solution and sodium formate solution are obtained; the obtained sodium formate solution is fed into the drier to be dried to obtain the sodium formate with the content being 97 percent; and meanwhile, the obtained pentaerythritol solution is added into water and is pumped into a crystallizing tank to raise the temperature so that the pentaerythritol is sufficiently dissolved, then, the temperature is lowered so that pentaerythritol crystals are separated out, and the pentaerythritol is obtained through recovery.
Description
Technical field
The present invention relates to a kind of preparation technology of tetramethylolmethane, relate in particular to a kind of method that from pentaerythrite mother liquor, reclaims useful matter such as tetramethylolmethane and sodium formiate.
Background technology
Traditional use sodium legal system is got tetramethylolmethane; After producing tetramethylolmethane, obtain to contain the pentaerythrite mother liquor of a large amount of sodium formiates, remaining tetramethylolmethane etc., can obtain sodium formiate through this pentaerythrite mother liquor being reclaimed separation, but because the restriction of tripping device and condition; The sodium formiate content of separating is about 93%; The moisture content of sodium formiate is controlled at about 1.5%, also has about 5.5% tetramethylolmethane not to be separated, and is present in the sodium formiate product with the form of impurity.Tetramethylolmethane one in the sodium formiate is the lifting that has a strong impact on the sodium formiate product content, the 2nd, and a large amount of tetramethylolmethanes is taken away by the sodium formiate product, and the sodium formiate price is brought serious economy loss well below the price of tetramethylolmethane to enterprise.The sodium formiate separating technology that adopts at present exists energy consumption big, and production cost is high, and the sodium formiate content of producing can not satisfy the demand in market, the defective of market competitiveness difference.
Sodium formiate is a kind of important organic raw material, has another name called sodium formate, and outward appearance is a white crystalline powder.Sodium formiate is widely used in printing and dyeing, chemical production field such as organic synthesis, medicine, and sodium formiate also is a main raw material of producing formic acid and oxalic acid, also is the raw material of producing vat powder.It can be used as the rawhide treatment agent of leather industry, the dye leveller of dope dyeing industry, the promotor of electroplating industry, the matting agent of Zantrel industry etc.About 200KT, owing to the coal resources reason, its industrial scale is received restriction, processing unit is backward, product is single, water power vapour cost high, lack competitive capacity according to the national sodium formiate ultimate production of report.
Analysis according to market; All there is certain vacancy in the market of sodium formiate derived product oxalic acid, vat powder, formic acid; Along with the huge demand in market will drive the bigger demand of sodium formiate product, the internationalization of produce market will require strict more to the sodium formiate quality product.Now on our market sodium formiate content generally at 91%, 93%, 95% 3 class.Given this sodium formiate content is further improved and reduce production costs enterprise's raising market competitiveness is had significant meaning.
Summary of the invention
The technical problem that the present invention will solve:
The present invention provides a kind of method that reclaims tetramethylolmethane and sodium formiate, can from pentaerythrite mother liquor, reclaim tetramethylolmethane and sodium formiate.Through this method, 93% thick sodium formiate is added water and sodium formiate mother liquor dissolve recentrifuge and purify to 97% elaboration sodium formiate.Can also be with centrifugal back mother liquor through adding water recrystallization, the centrifugal tetramethylolmethane that reclaims out, the mother liquor retrieval system behind the recentrifuge is made into the sodium formiate raw material again.Sub product sodium formiate production cost is low in the tetramethylolmethane production process, and can reach 97% through sodium formiate content after the technological transformation, and the waste liquid in the sodium formiate sepn process is realized zero release simultaneously, for realizing that the performance of enterprises has significant meaning.
Amount of water when how to control lixator dissolving mixed solution among the present invention is important, and the purpose that adds water is in order to regulate the proportion of sedimentation liquid, to regulate its viscosity and buoyancy through regulating proportion, finally obtaining quality clear liquid preferably.The quality of clear liquid refers to SF: PE: (CPE), SF content is high for DPE, TPE, and other two types of content are just low more, and the quality of clear liquid is just good more.It comprises solid and two aspects of solution: from solid phase, it is many more to add water, and proportion is low more, and buoyancy is more little, and sedimentation is good more, and (sedimentation refers to gravity and the two comparison of buoyancy of crystalline particle: gravity＞buoyancy, sinking; Gravity＜buoyancy, come-up; Gravity=buoyancy becomes suspension-s); From solution, it is more to add water, PE, and (CPE) dissolving of these two types of materials increases for DPE, TPE, and quality degenerates, thereby should select and control an an amount of amount of water.Recovery adds water can reduce material viscosity, reclaims good the drying, moreover can dissolve the part sodium formiate, improves and reclaims season alcohol quality.
Should also be noted that among the present invention and reclaim crystallization and reclaim centrifugal control after the recovery Tc dropped to specified temperature, whether switch put in place the inspection related valve earlier; Blow with steam and to thread a pipe; Add on request and open pump behind the water and begin to beat circulation, observe the internal circulating load size, the strict Control Circulation time.Although blow the clout road in, prevent the material plugging to the back termination of pumping cycling time, closed related valve, continue to be cooled to begin after the specified temperature centrifugal.Temperature is crossed the bad drying of low back reclaimed materials, and SF separates out and influence the reclaimed materials quality, and then influences single cropping content in the wash water, finally influences season pure output and quality.Temperature is too high, season alcohol separate out insufficiently, reclaim low, a large amount of season alcohol enrichment in system of yield, finally can cause the whole production system collapse.
Centrifugal easy race material makes and reclaims season alcohol yield and reduce, part season alcohol through mother liquor stream to the back workshop section, make and filter load and increase, and season alcohol output can decrease.Can cause the whole production system collapse after season, alcohol content increased in the mother liquor.
The Comprehensive Control of above-mentioned factor also is from pentaerythrite mother liquor, to extract sodium formiate and the importance that reclaims tetramethylolmethane.
The present invention is achieved in that
A kind of method that reclaims tetramethylolmethane and sodium formiate comprises the steps:
(1) pentaerythrite mother liquor is sent in the vaporizer evaporated;
(2) will carry out centrifugally through the mixed solution that evaporation obtains, obtain sodium formiate coarse fodder and sodium formiate mother liquor;
(3) the sodium formiate coarse fodder that step (2) is obtained carries out drying, obtains content and be 93% sodium formiate;
(4) content that the sodium formiate mother liquor that accounts for total amount 60% that obtains in the step (2) and step (3) is obtained is that 93% sodium formiate mixed solution is delivered to lixator, and adds entry, and wherein, the ratio of water and mixed solution is 4: 1, and mixed solution is stirred and fully dissolving;
(5) mixed solution that obtains in the step (4) is carried out once more centrifugal, obtain tetramethylolmethane solution and sodium formate solution;
(6) sodium formate solution that obtains in the step (5) is carried out drying, obtain content and be 97% sodium formiate.
The mixed solution that the residue that step (2) is obtained accounts for the sodium formiate mother liquor of total amount 40% returns in the mixed solution in the step (1) and recycles.
The tetramethylolmethane solution that obtains in the step (5) is added entry squeeze into crystallizer and heat up tetramethylolmethane is fully dissolved, the back cooling is separated out crystals of pentaerythritol, reclaims and obtains tetramethylolmethane.
The invention has the beneficial effects as follows:
Through method provided by the invention, through reclaiming the secondary centrifuging mode, the sub product sodium formiate content that produces in the tetramethylolmethane production process is promoted to 97% from 93%, this is a kind of novel purifying technique; Simultaneously, through adding water recrystallization, the centrifugal tetramethylolmethane that reclaims out, the mother liquor behind the recentrifuge can also retrieval system be made into the sodium formiate raw material again with this centrifugal back mother liquor.This compares with traditional purifying formic acid sodium from tetramethylolmethane, and this system has realized the raising of sodium formiate purity on the one hand, also realized the recycle of raw material on the other hand, and this technical process is simple, and is workable, is worthy to be popularized.
Description of drawings
Fig. 1 is the schema of the recovery method of pentaerythrite mother liquor of the present invention.
Embodiment
Embodiment
Utilizing scale is that 30,000 tons of/year tetramethylolmethane production equipments extract sodium formiate and reclaim tetramethylolmethane.
(1) pentaerythrite mother liquor is sent in the vaporizer,, evaporated most of moisture in the mixed solution through evaporation;
(2) will send into whizzer through the mixed solution that evaporation obtains and carry out centrifugally, obtain to obtaining sodium formiate coarse fodder and sodium formiate mother liquor;
The sodium formiate mother liquor mixed solution that accounts for total amount 40% that step (2) is obtained returns in the mixed solution in the step (1) and recycles.
(3) the sodium formiate coarse fodder that step (2) is obtained is sent into moisture eliminator and is carried out drying, obtains content and be 93% sodium formiate;
(4) content that the sodium formiate mother liquor that accounts for total amount 60% that obtains in the step (2) and step (3) is obtained is that 93% sodium formiate mixed solution is delivered to lixator, and adds entry, and wherein, the ratio of water and mixed solution is 4: 1, and mixed solution is stirred and fully dissolving; Recovery adds water and is used for reducing material viscosity on the one hand, reclaims good the drying, on the other hand, can the control section sodium formiate, improve and reclaim the tetramethylolmethane quality;
(5) mixed solution that obtains in the step (4) is sent into whizzer and carry out centrifugally once more, obtain tetramethylolmethane solution and sodium formate solution;
The tetramethylolmethane solution that obtains in the step (5) is added entry squeeze into crystallizer and heat up tetramethylolmethane is fully dissolved, the back cooling is separated out crystals of pentaerythritol, reclaims the tetramethylolmethane that obtains; The recovery that all can influence tetramethylolmethane too high or too low for temperature;
(6) sodium formate solution that obtains in the step (5) is sent into moisture eliminator and carry out drying, obtain content and be 97% sodium formiate.
Although disclose specific embodiment of the present invention and accompanying drawing for the purpose of illustration; Its purpose is to help to understand content of the present invention and implement according to this; But it will be appreciated by those skilled in the art that: in the spirit and scope that do not break away from the present invention and appended claim, various replacements, variation and modification all are possible.Therefore, the present invention should not be limited to most preferred embodiment and the disclosed content of accompanying drawing, and the scope that the present invention requires to protect is as the criterion with the scope that claims define.
Claims (2)
1. a method that reclaims tetramethylolmethane and sodium formiate comprises the steps:
(1) pentaerythrite mother liquor is sent in the vaporizer evaporated;
(2) will send into whizzer through the mixed solution that evaporation obtains and carry out centrifugally, obtain sodium formiate coarse fodder and sodium formiate mother liquor;
(3) the sodium formiate coarse fodder that step (2) is obtained is sent into moisture eliminator and is carried out drying, obtains content and be 93% sodium formiate;
(4) content that the sodium formiate mother liquor that accounts for total amount 60% that obtains in the step (2) and step (3) is obtained is that 93% sodium formiate mixed solution is delivered to lixator, and adds entry, and wherein, the ratio of water and mixed solution is 4: 1, and mixed solution is stirred and fully dissolving;
(5) mixed solution that obtains in the step (4) is sent into whizzer and carry out centrifugally once more, obtain tetramethylolmethane solution and sodium formate solution;
(6) sodium formate solution that obtains in the step (5) is sent into moisture eliminator and carry out drying, obtain content and be 97% sodium formiate;
(7) the tetramethylolmethane solution that obtains in the step (5) is added entry and squeeze into crystallizer and heat up tetramethylolmethane is fully dissolved, the back cooling is separated out crystals of pentaerythritol, reclaims and obtains tetramethylolmethane.
2. the method for recovery tetramethylolmethane according to claim 1 and sodium formiate is characterized in that, the sodium formiate mother liquor that accounts for total amount 40% that step (2) is obtained returns in the mother liquor in the step (1) and recycles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100547921A CN102617323A (en) | 2012-03-05 | 2012-03-05 | Method for recovering pentaerythritol and sodium formate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100547921A CN102617323A (en) | 2012-03-05 | 2012-03-05 | Method for recovering pentaerythritol and sodium formate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102617323A true CN102617323A (en) | 2012-08-01 |
Family
ID=46557593
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012100547921A Pending CN102617323A (en) | 2012-03-05 | 2012-03-05 | Method for recovering pentaerythritol and sodium formate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102617323A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103483178A (en) * | 2013-08-29 | 2014-01-01 | 烟台大学 | Method of treating waste residue in production of neopentyl glycol |
| CN103570522A (en) * | 2013-11-01 | 2014-02-12 | 安徽金禾实业股份有限公司 | Method for producing 99.5% of sodium formate |
| RU2604375C1 (en) * | 2015-09-22 | 2016-12-10 | Публичное акционерное общество "Метафракс" | Method of extracting sodium formiate from pentaerythritol-formiate mother solution |
| CN108558601A (en) * | 2018-06-19 | 2018-09-21 | 濮阳市永安化工有限公司 | Pentaerythrite separation mother liquor prepares the device and preparation method thereof of liquid pentaerythrite |
| CN111056938A (en) * | 2019-12-24 | 2020-04-24 | 赤峰瑞阳化工有限公司 | Purification method and purification device for pentaerythritol byproduct crude sodium formate |
| CN112745214A (en) * | 2021-02-14 | 2021-05-04 | 华东理工大学 | Method for separating and purifying sodium formate from pentaerythritol mother liquor by adopting solid phase extraction-elution crystallization method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4277620A (en) * | 1980-02-29 | 1981-07-07 | Virginia Chemicals Inc. | Byproduct recovery from a pentaerythritol waste stream |
| CS276064B6 (en) * | 1988-11-24 | 1992-03-18 | Palo Ondrej | Process for treating reaction solutions of pentaerythritol |
| CN1254702A (en) * | 1998-11-21 | 2000-05-31 | 衡阳三化实业股份有限公司 | Process for recovering pentaerythritol and protan from mother liquid of pentaerythritol |
| RU2199518C1 (en) * | 2001-10-04 | 2003-02-27 | Открытое акционерное общество "Химпласт" | Method for simultaneous production of pentaerythritol and sodium formate |
| CN102115358A (en) * | 2010-12-29 | 2011-07-06 | 王莉 | Method for producing pentaerythritol and sodium formate with waste liquor generated during preparation of pentaerythritol |
-
2012
- 2012-03-05 CN CN2012100547921A patent/CN102617323A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4277620A (en) * | 1980-02-29 | 1981-07-07 | Virginia Chemicals Inc. | Byproduct recovery from a pentaerythritol waste stream |
| CS276064B6 (en) * | 1988-11-24 | 1992-03-18 | Palo Ondrej | Process for treating reaction solutions of pentaerythritol |
| CN1254702A (en) * | 1998-11-21 | 2000-05-31 | 衡阳三化实业股份有限公司 | Process for recovering pentaerythritol and protan from mother liquid of pentaerythritol |
| RU2199518C1 (en) * | 2001-10-04 | 2003-02-27 | Открытое акционерное общество "Химпласт" | Method for simultaneous production of pentaerythritol and sodium formate |
| CN102115358A (en) * | 2010-12-29 | 2011-07-06 | 王莉 | Method for producing pentaerythritol and sodium formate with waste liquor generated during preparation of pentaerythritol |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103483178A (en) * | 2013-08-29 | 2014-01-01 | 烟台大学 | Method of treating waste residue in production of neopentyl glycol |
| CN103483178B (en) * | 2013-08-29 | 2015-10-21 | 烟台大学 | The method of process waste residue in production of neopentyl glycol |
| CN103570522A (en) * | 2013-11-01 | 2014-02-12 | 安徽金禾实业股份有限公司 | Method for producing 99.5% of sodium formate |
| CN103570522B (en) * | 2013-11-01 | 2015-11-18 | 安徽金禾实业股份有限公司 | A kind of production method of 99.5% sodium formiate |
| RU2604375C1 (en) * | 2015-09-22 | 2016-12-10 | Публичное акционерное общество "Метафракс" | Method of extracting sodium formiate from pentaerythritol-formiate mother solution |
| CN108558601A (en) * | 2018-06-19 | 2018-09-21 | 濮阳市永安化工有限公司 | Pentaerythrite separation mother liquor prepares the device and preparation method thereof of liquid pentaerythrite |
| CN111056938A (en) * | 2019-12-24 | 2020-04-24 | 赤峰瑞阳化工有限公司 | Purification method and purification device for pentaerythritol byproduct crude sodium formate |
| CN112745214A (en) * | 2021-02-14 | 2021-05-04 | 华东理工大学 | Method for separating and purifying sodium formate from pentaerythritol mother liquor by adopting solid phase extraction-elution crystallization method |
| CN112745214B (en) * | 2021-02-14 | 2022-12-20 | 华东理工大学 | Method for separating and purifying sodium formate from pentaerythritol mother liquor |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102617323A (en) | Method for recovering pentaerythritol and sodium formate | |
| CN104312627B (en) | A kind of crystallization process removes solvent and the method for resin in montanin wax | |
| WO2013091403A1 (en) | Method for producing potassium chloride, sodium chloride and magnesium sheets by brine mining from carnallite mine | |
| CN104109078B (en) | A kind of method that in Sulpyrine production, ethanol reclaims | |
| CN105668651A (en) | Production method for cobaltous sulfate heptahydrate | |
| CN101314609B (en) | Process for preparing D-glucosamine hydrochlorate | |
| CN112110462B (en) | Method for producing battery-grade lithium hydroxide by continuous freezing and dialysis crystallization mode | |
| CN103570523B (en) | A kind of production method of 95% sodium formiate | |
| CN102352054A (en) | Recovery process of solvent in polyphenylene sulfide resin production process | |
| CN105218317A (en) | A kind of method that in hexanitrobibenzyl production, ethanol reclaims and device | |
| CN104193634B (en) | A kind of separation of ammonia guanidine-acetic acid and the method for ammonium chloride mixed crystal | |
| CN104130105B (en) | The method that in D-4-methylsulfonylphserine serine ethyl ester production, ethanol is recycled | |
| CN113666393A (en) | Potassium chloride refining process and production system | |
| CN112724106A (en) | Synthetic method of high-purity TGDDM epoxy resin | |
| CN204039299U (en) | A kind of purifying plant of high-purity sodium formate | |
| CN102746134A (en) | Method for decreasing content of sodium chloride impurities in recovered sodium formate | |
| CN106928172A (en) | A kind of process for refining of dibenzofuran | |
| CN110194715A (en) | A kind of production method of sodium formate | |
| CN111848453B (en) | Production process and production line of 4-methyl-2' -cyanobiphenyl | |
| CN202440450U (en) | System for extracting sodium formate generated in pentaerythritol | |
| CN101845038B (en) | Method and device for processing lactide refined raffinate | |
| CN103570522A (en) | Method for producing 99.5% of sodium formate | |
| CN111807949A (en) | Method for recovering ibuprofen sodium salt from ibuprofen sodium salt mother liquor | |
| CN205832669U (en) | A kind of system of recovered material from crystallization feed liquid | |
| CN100506763C (en) | Method for purifying biphenyl by elution crystallization |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| AD01 | Patent right deemed abandoned |
Effective date of abandoning: 20120801 |
|
| C20 | Patent right or utility model deemed to be abandoned or is abandoned |