CN102516061A - Processing method and processing device of crylic acid and ester heavy components - Google Patents
Processing method and processing device of crylic acid and ester heavy components Download PDFInfo
- Publication number
- CN102516061A CN102516061A CN2011103907765A CN201110390776A CN102516061A CN 102516061 A CN102516061 A CN 102516061A CN 2011103907765 A CN2011103907765 A CN 2011103907765A CN 201110390776 A CN201110390776 A CN 201110390776A CN 102516061 A CN102516061 A CN 102516061A
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- Prior art keywords
- vinylformic acid
- heavy constituent
- spiral pyrolyzer
- spiral
- pyrolyzer
- 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.)
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- 150000002148 esters Chemical class 0.000 title claims abstract description 35
- 239000002253 acid Substances 0.000 title abstract 7
- 238000003672 processing method Methods 0.000 title abstract 3
- 238000000034 method Methods 0.000 claims abstract description 36
- 230000008569 process Effects 0.000 claims abstract description 24
- 238000004821 distillation Methods 0.000 claims abstract description 19
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 76
- 239000000470 constituent Substances 0.000 claims description 39
- 239000000463 material Substances 0.000 claims description 22
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000005336 cracking Methods 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 6
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 4
- 230000008676 import Effects 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 2
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 2
- 230000007774 longterm Effects 0.000 abstract 1
- 238000011084 recovery Methods 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- CYUZOYPRAQASLN-UHFFFAOYSA-N 3-prop-2-enoyloxypropanoic acid Chemical compound OC(=O)CCOC(=O)C=C CYUZOYPRAQASLN-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 235000019628 coolness Nutrition 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- -1 stopper Chemical compound 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A processing method of crylic acid and ester heavy components includes the following steps: A) conducting distillation splitting on the crylic acid or the ester heavy components to enable the crylic acid or the ester heavy components to be converted into crylic acid steam; B) condensing and collecting the crylic acid steam; and C) purifying the collected crylic acid. The processing method is simple in process flow, high in recycle rate, high in purity, stable in long-term operation, capable of bringing high economical and environment benefits to society and worth popularizing in the market.
Description
Technical field
The invention belongs to the chemical industry environmental protection field, relate to a kind of vinylformic acid and ester class heavy constituent treatment process particularly.
The invention still further relates to the device of realizing aforesaid method.
Background technology
Vinylformic acid and ester class thereof are developed rapidly as the essential industry derived prods of propylene in recent years, have greatly enriched people's life.But having a large amount of vinylformic acid or esters of acrylic acid heavy constituent in the production process produces.Waste oil is also claimed in the vinylformic acid heavy constituent; Be meant that the weight-removing column still goes out; Residue through after the vinylformic acid recovery system processing of being made up of dimer decomposer and thin-film evaporator mainly contains acrylic acid dimer, stopper, toxilic acid, a small amount of vinylformic acid and some other heavy component.The heavy constituent of propenoate are the reaction kettle bed materials, mainly contain the oligopolymer of vinylformic acid and propenoate, and a certain amount of vinylformic acid and propenoate are arranged in addition.
The treatment process of vinylformic acid and the heavy constituent of ester class mainly contains two kinds at present: a kind of is to burn harmless treatment, has caused the wasting of resources; Another kind is the outer ERM processing of selling qualification, but processing costs is higher or reclaim not thorough.Therefore be badly in need of a kind of new technology with vinylformic acid and ester class heavy constituent resource utilization, can be from heavy constituent heavy metals such as acrylic acid, propenoate and cobalt, manganese.
Summary of the invention
The object of the present invention is to provide a kind of vinylformic acid and ester class heavy constituent treatment process.
Another purpose of the present invention is to provide a kind of device of realizing aforesaid method.
The present invention adopts and to be suitable for the vinylformic acid in high boiling point, the abundant acrylic acid of full-bodied spiral pyrolyzer and the heavy constituent of ester class, and it is simple to have a technical process, and the recovery is high, and purity is high, the characteristics that long-time running is stable.
For realizing above-mentioned purpose, the treatment process of vinylformic acid provided by the invention and the heavy constituent of ester class may further comprise the steps:
A) vinylformic acid or the heavy constituent of ester class are distilled cracking and are changed vinylformic acid steam into;
B) vinylformic acid steam is collected after condensation;
C) vinylformic acid of collecting is purified.
Described treatment process, wherein, vinylformic acid in the steps A or the heavy constituent of ester class are vinylformic acid and the heavy constituent of ester class in the production workshop section.
Described treatment process, wherein, the horizontal spiral pyrolyzer is adopted in the distillation cracking, and by basic, normal, high three isolating cuts of temperature section Fractional Collections.
Described treatment process, wherein, normal pressure or underpressure distillation are adopted in the distillation cracking.
Described treatment process, wherein, vinylformic acid heavy constituent distillation temperature is 140～160 ℃.
Described treatment process, wherein, esters of acrylic acid heavy constituent distillation temperature is 110～225 ℃.
Described treatment process, wherein, esters of acrylic acid is methyl acrylate, ethyl propenoate or Bing Xisuandingzhi.
The spiral pyrolyzer that is used to realize aforesaid method provided by the invention, its structure is:
The conveying lever of convey materials surface is a helicoidal structure in the spiral pyrolyzer; The conveying lever of spiral pyrolyzer is by electric motor driving.
One end on spiral pyrolyzer top is provided with material inlet; And be respectively arranged with in turn on spiral pyrolyzer top that low-temperature zone is collected mouthful, middle-temperature section is collected mouthful and high temperature section is collected mouthful; Low-temperature zone is collected mouth near material inlet; High temperature section collection mouth is located at the other end of spiral pyrolyzer, and middle-temperature section collection mouth is collected between the mouth at low-temperature zone collection mouth and high temperature section;
The other end bottom of the corresponding material inlet of spiral pyrolyzer is provided with material outlet;
The two ends of spiral pyrolyzer are respectively equipped with a heating agent import and heating agent outlet;
Spiral pyrolyzer outside has one deck that material is heated the heating jacket of thermal medium is housed uniformly.
Described spiral pyrolyzer, wherein, the conveying lever of spiral pyrolyzer is driven through speed reduction unit by motor.
Technical process of the present invention is simple, and normal pressure or decompression distillation does not down need plus solvent; The vinylformic acid recovery is high, and purity is high, and long-time running is stable; Can be for society bring very high economic benefit and social benefit, be a kind of vinylformic acid that is worth on market, promoting and the method for ester class heavy constituent resource utilization.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Fig. 2 is a spiral cracking furnace installation synoptic diagram.
Element numbers explanation in the accompanying drawing:
1 storage tank, 2 spiral pyrolyzer, 3 condenser systems, 4 run tanks, 5 rectifying tower, 6 recycling ponds, 7 residue scoops, 8 motors, 9 step-down gears, 10 material inlets, 11 low-temperature zone are collected mouth, 12 middle-temperature sections are collected mouth, 13 high temperature section collection mouth, 14 material outlets, 15 heating jackets, 16 heating agent imports, the outlet of 17 heating agents;
Embodiment
Technical scheme of the present invention may further comprise the steps:
A) vinylformic acid in the collection production workshop section or the heavy constituent of ester class are to storage tank;
B) vinylformic acid or the heavy constituent of ester class are sent in the spiral pyrolyzer, distill cracking, and residual vinylformic acid changes vinylformic acid steam into;
C) vinylformic acid steam is through the condenser system condensation;
D) get into run tank then, residual residue pushes the residue scoop;
E) vinylformic acid entering rectifying tower is purified in the run tank, obtains high purity acrylic acid and recycles.
The method of said vinylformic acid and ester class heavy constituent resource utilization, wherein, the spiral pyrolyzer adopts horizontal, and is divided into basic, normal, high three temperature sections heating, and Fractional Collections separate fraction, sped structure are easier to the removing of residue;
The method of said vinylformic acid and ester class heavy constituent resource utilization, wherein, still-process can adopt normal pressure or underpressure distillation in the spiral pyrolyzer.
The method of said vinylformic acid and ester class heavy constituent resource utilization, wherein, vinylformic acid heavy constituent distillation temperature is 140～160 ℃, the residence time is 3～5h.
The method of said vinylformic acid and ester class heavy constituent resource utilization, wherein, vinylformic acid purity is up to 98% in the vinylformic acid heavy constituent separate fraction, and the vinylformic acid recovery is 99%.
The method of said vinylformic acid and ester class heavy constituent resource utilization, wherein, esters of acrylic acid heavy constituent distillation temperature is 110～225 ℃, the residence time is 2～4h.
The method of said vinylformic acid and ester class heavy constituent resource utilization, wherein, esters of acrylic acid heavy constituent separate fraction vinylformic acid purity is 79%, the vinylformic acid recovery is 99%.
Below enumerate several embodiment effect of the present invention is described, but claim scope of the present invention is not limited only to this.
Embodiment 1
The vinylformic acid heavy constituent derive from certain vinylformic acid manufacturing enterprise, and sample is the black viscous liquid, and viscous modulus is bigger, and have certain irritating smell, collect to be placed in the storage tank 1.Spiral pyrolyzer 2 is sent in the heavy constituent of 1000g vinylformic acid, elevated temperature to 140～160 ℃, distillation cracking 5h; Get into run tank 4 through condenser system 3 coolings; Acrylic acid concentration adopts the gas chromatography mass spectrometry chromatographic determination in the cut, is 98% through calculating vinylformic acid purity, after rectifying tower 5 is purified to high purity acrylic acid, gets into then to recycle in the pond 6 (to purify and be high purity acrylic acid 673g; The vinylformic acid recovery is 99%), the residue after the distillation cracking gets into residue scoop 7.Whole technology need not add any solvent, and flow process is simple, and the recovery is high, has high economic benefit and social benefit.
The structure of spiral pyrolyzer 2 of the present invention is seen shown in Figure 2, and the spiral pyrolyzer mainly is made up of motor, step-down gear and body of heater, and the spiral pyrolyzer adopts horizontal use, to increase the service life.
The conveying lever of convey materials surface is a helicoidal structure in the spiral pyrolyzer 2, when convey materials, is difficult for sizing, and residue is easy to remove, and has also effectively guaranteed the high heat transfer coefficient of equipment.The conveying lever of spiral pyrolyzer is driven through speed reduction unit 9 by motor 8.
One end on spiral pyrolyzer top is provided with material inlet 10; And be respectively arranged with in turn on spiral pyrolyzer top that low-temperature zone collects mouthfuls 11, middle-temperature section collect mouthfuls 12 and high temperature section collect mouthfuls 13; Low-temperature zone is collected mouth 11 near material inlet 10; High temperature section collection mouth 13 is opened in the other end of spiral pyrolyzer, and middle-temperature section collection mouth 12 is collected between mouth 11 and the high temperature section collection mouth 13 in low-temperature zone.
The other end bottom of spiral pyrolyzer 2 corresponding material inlets 10 is provided with material outlet 14.
The two ends of spiral pyrolyzer 2 be respectively equipped with a heating agent import 16 and heating agent outlet 17 (heating agent be deep fat or (with) steam).
The Bing Xisuandingzhi heavy constituent derive from certain vinylformic acid manufacturing enterprise, and sample is a black liquor, and certain irritating smell is arranged.The spiral pyrolyzer is sent in the heavy constituent of 1000g Bing Xisuandingzhi, elevated temperature to 170～225 ℃, distillation cracking 3h; Get into run tank through the condenser system cooling; Acrylic acid concentration adopts the gas chromatography mass spectrometry chromatographic determination in the cut, is 79% through calculating vinylformic acid purity, and purifying through rectifying tower then is high purity acrylic acid 559g; Acrylic acid recovery is 99%, and the residue after the distillation cracking gets into the residue scoop.Whole technology need not add any solvent, and flow process is simple, and the recovery is high, has high economic benefit and social benefit.
Claims (9)
1. the treatment process of vinylformic acid and the heavy constituent of ester class may further comprise the steps:
A) vinylformic acid or the heavy constituent of ester class are distilled cracking and are changed vinylformic acid steam into;
B) vinylformic acid steam is collected after condensation;
C) vinylformic acid of collecting is purified.
2. treatment process according to claim 1, wherein, vinylformic acid in the steps A or the heavy constituent of ester class are vinylformic acid or the heavy constituent of ester class in the production workshop section.
3. treatment process according to claim 1, wherein, the horizontal spiral pyrolyzer is adopted in the distillation cracking, and by basic, normal, high three isolating cuts of temperature section Fractional Collections.
4. treatment process according to claim 1, wherein, normal pressure or underpressure distillation are adopted in the distillation cracking.
5. treatment process according to claim 1, wherein, vinylformic acid heavy constituent distillation temperature is 140～160 ℃, the residence time is 3～5h.
6. treatment process according to claim 1, wherein, esters of acrylic acid heavy constituent distillation temperature is 110～225 ℃, the residence time is 2～4h.
7. according to claim 1 or 6 described treatment processs, wherein, esters of acrylic acid is methyl acrylate, ethyl propenoate or Bing Xisuandingzhi.
8. spiral pyrolyzer of realizing the said method of claim 1, its structure is:
The conveying lever of convey materials surface is a helicoidal structure in the spiral pyrolyzer; The conveying lever of spiral pyrolyzer is by electric motor driving;
One end on spiral pyrolyzer top is provided with material inlet; And be respectively arranged with in turn on spiral pyrolyzer top that low-temperature zone is collected mouthful, middle-temperature section is collected mouthful and high temperature section is collected mouthful; Low-temperature zone is collected mouth near material inlet; High temperature section collection mouth is located at the other end of spiral pyrolyzer, and middle-temperature section collection mouth is collected between the mouth at low-temperature zone collection mouth and high temperature section;
The other end bottom of the corresponding material inlet of spiral pyrolyzer is provided with material outlet;
The two ends of spiral pyrolyzer are respectively equipped with a heating agent import and heating agent outlet;
Spiral pyrolyzer outside has one deck that material is heated the heating jacket of thermal medium is housed uniformly.
9. spiral pyrolyzer according to claim 8, wherein, the conveying lever of spiral pyrolyzer is driven through speed reduction unit by motor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103907765A CN102516061A (en) | 2011-11-30 | 2011-11-30 | Processing method and processing device of crylic acid and ester heavy components |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103907765A CN102516061A (en) | 2011-11-30 | 2011-11-30 | Processing method and processing device of crylic acid and ester heavy components |
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| Publication Number | Publication Date |
|---|---|
| CN102516061A true CN102516061A (en) | 2012-06-27 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011103907765A Pending CN102516061A (en) | 2011-11-30 | 2011-11-30 | Processing method and processing device of crylic acid and ester heavy components |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557510A (en) * | 2014-12-04 | 2015-04-29 | 江门谦信化工发展有限公司 | Method for recovering butyl acrylate polymer |
| CN104557538A (en) * | 2014-12-04 | 2015-04-29 | 江门谦信化工发展有限公司 | Industrial production method for producing butyl acrylate by in-column reaction rectification |
| CN111362786A (en) * | 2018-12-25 | 2020-07-03 | 万华化学集团股份有限公司 | Method for recycling methyl acrylate heavy component |
| CN114907030A (en) * | 2022-05-26 | 2022-08-16 | 昌德新材科技股份有限公司 | Cement raw material additive and application thereof and cement production process |
| CN114920489A (en) * | 2022-05-26 | 2022-08-19 | 昌德新材科技股份有限公司 | Cement raw material additive, application thereof and cement production process |
| CN114956645A (en) * | 2022-05-26 | 2022-08-30 | 昌德新材科技股份有限公司 | Slag grinding aid and application thereof |
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| CN1907942A (en) * | 2006-07-28 | 2007-02-07 | 沈福昌 | Treatment method of acrylic acid and esters waste oil resource |
| CN2903043Y (en) * | 2006-04-25 | 2007-05-23 | 大庆油田创业集团有限公司 | A cracking device for harmless treatment of oily sludge and sand |
| CN201825890U (en) * | 2010-10-21 | 2011-05-11 | 淄博市兴鲁化工有限公司 | Semi-continuous acrylic waste oil cracking device |
-
2011
- 2011-11-30 CN CN2011103907765A patent/CN102516061A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2903043Y (en) * | 2006-04-25 | 2007-05-23 | 大庆油田创业集团有限公司 | A cracking device for harmless treatment of oily sludge and sand |
| CN1907942A (en) * | 2006-07-28 | 2007-02-07 | 沈福昌 | Treatment method of acrylic acid and esters waste oil resource |
| CN201825890U (en) * | 2010-10-21 | 2011-05-11 | 淄博市兴鲁化工有限公司 | Semi-continuous acrylic waste oil cracking device |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557510A (en) * | 2014-12-04 | 2015-04-29 | 江门谦信化工发展有限公司 | Method for recovering butyl acrylate polymer |
| CN104557538A (en) * | 2014-12-04 | 2015-04-29 | 江门谦信化工发展有限公司 | Industrial production method for producing butyl acrylate by in-column reaction rectification |
| CN111362786A (en) * | 2018-12-25 | 2020-07-03 | 万华化学集团股份有限公司 | Method for recycling methyl acrylate heavy component |
| CN114907030A (en) * | 2022-05-26 | 2022-08-16 | 昌德新材科技股份有限公司 | Cement raw material additive and application thereof and cement production process |
| CN114920489A (en) * | 2022-05-26 | 2022-08-19 | 昌德新材科技股份有限公司 | Cement raw material additive, application thereof and cement production process |
| CN114956645A (en) * | 2022-05-26 | 2022-08-30 | 昌德新材科技股份有限公司 | Slag grinding aid and application thereof |
| CN114920489B (en) * | 2022-05-26 | 2024-02-09 | 昌德新材科技股份有限公司 | Cement raw material additive and application thereof and cement production process |
| CN114956645B (en) * | 2022-05-26 | 2024-02-13 | 昌德新材科技股份有限公司 | Slag grinding aid and application thereof |
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Application publication date: 20120627 |