CN1258668A - Method of recovering neopentyl diol from sodium formate as by product - Google Patents
Method of recovering neopentyl diol from sodium formate as by product Download PDFInfo
- Publication number
- CN1258668A CN1258668A CN 98126104 CN98126104A CN1258668A CN 1258668 A CN1258668 A CN 1258668A CN 98126104 CN98126104 CN 98126104 CN 98126104 A CN98126104 A CN 98126104A CN 1258668 A CN1258668 A CN 1258668A
- Authority
- CN
- China
- Prior art keywords
- neopentyl glycol
- dehydration
- still
- tower
- sodium formiate
- 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.)
- Granted
Links
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 title claims abstract description 30
- 239000006227 byproduct Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims description 17
- 239000004280 Sodium formate Substances 0.000 title abstract 4
- 235000019254 sodium formate Nutrition 0.000 title abstract 4
- -1 neopentyl diol Chemical class 0.000 title 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000000047 product Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000018044 dehydration Effects 0.000 claims description 37
- 238000006297 dehydration reaction Methods 0.000 claims description 37
- 230000009102 absorption Effects 0.000 claims description 20
- 238000010521 absorption reaction Methods 0.000 claims description 20
- 238000004821 distillation Methods 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- 241000209094 Oryza Species 0.000 claims description 10
- 235000007164 Oryza sativa Nutrition 0.000 claims description 10
- 235000009566 rice Nutrition 0.000 claims description 10
- 241000282326 Felis catus Species 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000000630 rising effect Effects 0.000 claims description 6
- 239000000945 filler Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 238000007790 scraping Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- DJOWTWWHMWQATC-KYHIUUMWSA-N Karpoxanthin Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1(O)C(C)(C)CC(O)CC1(C)O)C=CC=C(/C)C=CC2=C(C)CC(O)CC2(C)C DJOWTWWHMWQATC-KYHIUUMWSA-N 0.000 claims 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 238000009835 boiling Methods 0.000 abstract 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 16
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 8
- 235000019253 formic acid Nutrition 0.000 description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000013505 freshwater Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- AMIMRNSIRUDHCM-UHFFFAOYSA-N Isopropylaldehyde Chemical compound CC(C)C=O AMIMRNSIRUDHCM-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000004971 Cross linker Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
Sodium formate solution as by product of neopentyl glycol production is heated and dried to obtain sodium formate, evaporated steam and neopentyl glycol vapor is water adsorbed, dewatered and distilled to separate low boiling point matter and neopentyl glycol product, the low boiling point matter is returned to dewatering reactor for recovery and the neopentyl glycol product is cooled and scraped. The present invention can obtain high quality sodium formate with wide application.
Description
The invention discloses a kind of recovery technology of neopentyl glycol, particularly a kind of method that from neopentyl glycol by-product sodium formiate, reclaims neopentyl glycol.
Neopentyl glycol is to produce the raw material of saturated polyester resin, unsaturated polyester resin, powder coating, photosensitive crosslinker, Synolac.Industrial is to carry out condensation reaction with formaldehyde, isobutyric aldehyde in the presence of sodium hydroxide to generate neopentyl glycol and equimolar sodium formiate reaction solution.Reaction solution neutralizes with formic acid, obtains neopentyl glycol by-product sodium formiate after decompression stripping or solvent extraction neopentyl glycol.Stripping liquid or extraction liquid are through distillation dehydration (or solvent), and rectification under vacuum, scraping blade get the finished product neopentyl glycol.And the common neopentyl glycol of 4-8% and the moisture content of 5-8% of also containing in the neopentyl glycol by-product sodium formiate that obtains; prior art is to receive to react with sulfuric acid and neopentyl glycol by-product formic acid to produce formic acid; so consume high (because of its organism----mainly is a neopentyl glycol content height); 1 ton of formic acid of every production needs sodium formiate 2-2.1 ton; and can not obtain qualified formic acid; its purposes is restricted, and neopentyl glycol also fails to obtain effective recycling, has not only wasted resource but also contaminate environment.
The purpose of this invention is to provide that a kind of technology is simple, reduced investment, cost be low, not only recyclable neopentyl glycol but also can improve the method that reclaims neopentyl glycol from neopentyl glycol by-product sodium formiate of sodium formiate quality.
The technical scheme that realizes above-mentioned purpose of the present invention is: neopentyl glycol by-product sodium formiate is heated to 100-150 ℃ with steam, thermal oil, stack gas or other heat-conducting medium is dried to the sodium formiate solid under vacuum condition; The water vapor that evaporates is absorbed into absorption liquid with neopentyl glycol steam water in absorbing cylinder, comparatively complete in order to make absorption, reduce the loss of neopentyl glycol, can adopt one-level, secondary or three grades of absorptions; When the amount of neopentyl glycol containing in the one-level absorption liquid reaches 40-85%, it is sent into the dehydration of neopentyl glycol dehydration still internal heating normal pressure, on the dehydration still, the high dehydration tower of 2-6 rice is housed, filler is housed in the tower, the cat head terminal temperature is 105-135 ℃ in the dehydration; When the dehydration cat head reaches said temperature, material is evacuated to still kettle underpressure distillation (also can underpressure distillation in the dehydration still for saving investment), still kettle also is equipped with the high distillation tower of 2-6 rice, filler is housed in the tower, in order to improve the yield of neopentyl glycol, reduce the loss of neopentyl glycol, prevent that neopentyl glycol from entering vacuum pump, between finished product still and vacuum pump, absorption unit is housed, open vacuum pump and intensification, keep the still internal pressure between-0.08 to-0.092MPa, go out low-boiling-point substance when rising to 125-165 ℃, treat that tower top temperature goes out finished product when rising to 165-175 ℃ etc. tower top temperature, the finished product condenser temperature is controlled at 130-140 ℃, the gained finished product gets neopentyl glycol through the cooling scraping blade, and the residue in the still kettle excludes at the bottom of still, and low-boiling-point substance can return in the dehydration still and reclaim neopentyl glycol again.
The present invention adopts as above technical scheme, and it is simple to have technology, low equipment investment, the characteristics that cost is low; Can obtain high-quality sodium formiate: organic content＜0.5% in the dried sodium formiate, water content＜0.5% can be directly for the usefulness of producing formic acid; The consumption of producing formic acid with dried sodium formiate is low: formic acid consumption sodium formiate 1.45-1.55 ton per ton, and the recyclable 30-60 kilogram of sodium formiate per ton neopentyl glycol, quality product all can reach primary standard; The purposes of neopentyl glycol by-product sodium formiate is wide: because organic content is low in the sodium formiate of gained, also can be used for producing vat powder and oxalic acid; The present invention both can reduce environmental pollution, and can turn waste into wealth again economizes on resources, and has good social benefit and economic benefit.
Describe technical scheme of the present invention in detail below in conjunction with embodiment.
Embodiment 1: with 6 tons of neopentyl glycol by-product sodium formiates in three batches, 2 tons every batch are dropped into volume is 3.8m
3Rake type dryer in, under 10-15 rev/min of condition, under little band negative pressure, be heated to 100-150 ℃ with 0.3 to 0.7MPa steam and be dried to the sodium formiate powder.The water vapor that evaporates is absorbed into absorption liquid with neopentyl glycol steam with secondary; When the amount of neopentyl glycol containing in the one-level absorption liquid reaches 72% (being waxy solid during low temperature), it is sent into the dehydration of neopentyl glycol dehydration still internal heating normal pressure, again the secondary absorption liquid is put into one-level and absorbed cylinder, absorb two and replenish fresh water in the cylinder.In order to reduce the loss of neopentyl glycol in dehydration, on the dehydration still, the dehydration tower that diameter is 300mm is housed, filling material in the tower, tower height 3-4 rice; When the dehydration tower top temperature reaches 120-125 ℃, material is evacuated to underpressure distillation in the still kettle, the distillation tower that diameter is 300mm is housed on the still kettle, filler is housed, tower height 3-4 rice in the tower; In order to improve the yield of neopentyl glycol, between finished product still and vacuum pump, adorn an absorption unit, to reduce the loss of neopentyl glycol, prevent that neopentyl glycol from entering vacuum pump, open vacuum pump, keep the still internal pressure between-0.08 to-0.092MPa, treat that tower top temperature goes out low-boiling-point substance when rising to 125-165 ℃, treat that tower top temperature goes out finished product when rising to 165-175 ℃, the starting temperature that goes out finished product should not be low excessively, otherwise water content is difficult to qualifiedly in the finished product, and the finished product condenser temperature is controlled at 130-140 ℃, the meeting crystallization in condenser of the low finished product of finished product condenser temperature, the high finished product of temperature is not cold can to stop up vacuum pipe; Residue in the still kettle can exclude that (residue is the higher fuel of calorific value at the bottom of the still, but the boiler of feeding burning is used), go out the low-boiling-point substance that is gone out in the low-boiling-point substance process and can return dehydration and reclaim neopentyl glycol again in the still, go out the finished product that is gone out in the finished product process and get neopentyl glycol through the cooling scraping blade.Adopt the dry 6 tons of neopentyl glycol by-product sodium formiates of present method, recyclable altogether 205 kilograms of neopentyl glycol (product is first grade) and 5250 kilograms of sodium formiates, sodium formiate content 97%, organic content 0.4%, moisture 0.45%.
Embodiment 2: concrete grammar is with embodiment 1, but only adopts one-level to absorb, and promptly when the amount of neopentyl glycol containing in the one-level absorption liquid reaches 72%, it sent into the dehydration of dehydration still internal heating normal pressure, and add fresh water in one-level absorption cylinder.Adopt the dry 6 tons of neopentyl glycol by-product sodium formiates of present method, recyclable 120 kg neopentyl glycol.As seen the amount that adopts secondary to absorb the neopentyl glycol that reclaims absorbs greater than one-level.
Embodiment 3: concrete grammar is with embodiment 1, but adopt three grades of absorptions, promptly when the amount of neopentyl glycol containing in the one-level absorption liquid reaches 72%, it is sent into the dehydration of dehydration still heating normal pressure, the secondary absorption liquid is put into one-level absorb cylinder, three grades of absorption liquids are put into secondary absorb cylinder, and add fresh water to three grades of absorption cylinders; And for the save design investment, save still kettle, directly underpressure distillation in the dehydration still, be that dehydration finishes just to begin to carry out distillation procedure in the dehydration still, because dehydration and distillation are carried out in same equipment, so every batch of time will prolong 8 hours, its quality is with embodiment 1, but yield is than embodiment 1 height.
Claims (8)
1, a kind of method that reclaims neopentyl glycol from neopentyl glycol by-product sodium formiate is characterized in that neopentyl glycol by-product sodium formiate is heated to 100-150 ℃ with heat-conducting medium under vacuum condition be dried to the sodium formiate solid; The water vapor that evaporates is absorbed into absorption liquid with neopentyl glycol steam water in absorbing cylinder, can adopt one-level, secondary or three grades of absorptions; When the amount of neopentyl glycol containing in the one-level absorption liquid reaches 40-85%, it is sent into the dehydration of neopentyl glycol dehydration still internal heating normal pressure, on the dehydration still, the high dehydration tower of 2-6 rice is housed, filler is housed in the tower, the cat head terminal temperature is 105-135 ℃ in the dehydration; When the dehydration cat head reaches said temperature, material is evacuated to the still kettle underpressure distillation, still kettle also is equipped with the high distillation tower of 2-6 rice, filler is housed in the tower, between finished product still and vacuum pump, absorption unit is housed, open vacuum pump and intensification, keep the still internal pressure between-0.08 to-0.092MPa, go out low-boiling-point substance when rising to 125-165 ℃ etc. tower top temperature, treat that tower top temperature goes out finished product when rising to 165-175 ℃, the finished product condenser temperature is controlled at 130-140 ℃, and the gained finished product gets neopentyl glycol through the cooling scraping blade; Residue in the still kettle excludes at the bottom of still, and low-boiling-point substance can return in the dehydration still and reclaim neopentyl glycol again.
2, the method that reclaims neopentyl glycol from neopentyl glycol by-product sodium formiate as claimed in claim 1, it is characterized in that can underpressure distillation in the dehydration still.
3, the method that reclaims neopentyl glycol from neopentyl glycol by-product sodium formiate as claimed in claim 1 or 2 is characterized in that new penta tetrol by-product sodium formiate is dried to the sodium formiate solid with the 0.3-0.7MPa steam heating in rake type dryer.
4, method as claimed in claim 1 or 2, the height that it is characterized in that dehydration tower is a 3-4 rice, the height of distillation tower also is a 3-4 rice.
5, method as claimed in claim 3, the height that it is characterized in that dehydration tower is a 3-4 rice, the height of distillation tower also is a 3-4 rice.
6,, it is characterized in that the cat head terminal temperature is 120-125 ℃ in the dehydration as claim 1 or 2 or 5 described methods.
7, method as claimed in claim 3 is characterized in that the cat head terminal temperature is 120-125 ℃ in the dehydration.
8, method as claimed in claim 4 is characterized in that the cat head terminal temperature is 120-125 ℃ in the dehydration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98126104 CN1114584C (en) | 1998-12-26 | 1998-12-26 | Method of recovering neopentyl diol from sodium formate as by product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98126104 CN1114584C (en) | 1998-12-26 | 1998-12-26 | Method of recovering neopentyl diol from sodium formate as by product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1258668A true CN1258668A (en) | 2000-07-05 |
| CN1114584C CN1114584C (en) | 2003-07-16 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 98126104 Expired - Fee Related CN1114584C (en) | 1998-12-26 | 1998-12-26 | Method of recovering neopentyl diol from sodium formate as by product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1114584C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103483179A (en) * | 2013-09-18 | 2014-01-01 | 烟台大学 | Method for purifying crude sodium formate byproduct from neopentyl glycol production |
| CN105175227A (en) * | 2015-09-01 | 2015-12-23 | 保定市国秀化工有限责任公司 | Method for increasing yield and purity of neopentyl glycol |
| CN106800498A (en) * | 2015-11-25 | 2017-06-06 | 衡阳屹顺化工有限公司 | A kind of process units of neopentyl glycol |
| CN107216248A (en) * | 2017-06-29 | 2017-09-29 | 宁夏海纳川化工技术有限公司 | A kind of technique for producing sodium oxalate with polynary alcohol production byproduct sodium formate |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101407447B (en) * | 2008-11-08 | 2012-06-27 | 浙江工业大学 | Efficient recovery method for neopentyl glycol |
-
1998
- 1998-12-26 CN CN 98126104 patent/CN1114584C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103483179A (en) * | 2013-09-18 | 2014-01-01 | 烟台大学 | Method for purifying crude sodium formate byproduct from neopentyl glycol production |
| CN103483179B (en) * | 2013-09-18 | 2015-04-15 | 烟台大学 | Method for purifying crude sodium formate byproduct from neopentyl glycol production |
| CN105175227A (en) * | 2015-09-01 | 2015-12-23 | 保定市国秀化工有限责任公司 | Method for increasing yield and purity of neopentyl glycol |
| CN106800498A (en) * | 2015-11-25 | 2017-06-06 | 衡阳屹顺化工有限公司 | A kind of process units of neopentyl glycol |
| CN107216248A (en) * | 2017-06-29 | 2017-09-29 | 宁夏海纳川化工技术有限公司 | A kind of technique for producing sodium oxalate with polynary alcohol production byproduct sodium formate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1114584C (en) | 2003-07-16 |
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