CN104177258A - Method for preparing vinyl acetate - Google Patents
Method for preparing vinyl acetate Download PDFInfo
- Publication number
- CN104177258A CN104177258A CN201310201504.5A CN201310201504A CN104177258A CN 104177258 A CN104177258 A CN 104177258A CN 201310201504 A CN201310201504 A CN 201310201504A CN 104177258 A CN104177258 A CN 104177258A
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- China
- Prior art keywords
- acetylene
- vinyl acetate
- acetic acid
- plastic
- preparation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/04—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides onto unsaturated carbon-to-carbon bonds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for preparing vinyl acetate. With acetic acid and acetylene as raw materials, the method is characterized by comprising the steps: pressurizing acetylene, then mixing and heating with acetic acid, and then carrying out a reaction, wherein the acetylene pressurized pressure is 0.04 MPa-0.07 MPa, the temperature before pressurization is 20-30 DEG C, and the temperature after pressurization is 20-60 DEG C. The safety pressure of acetylene can be improved, so that the acetylene per-pass conversion is improved to reach 12%-13%, and thus the production is greatly increased, the process flow is reduced and optimized, and energy consumption is reduced.
Description
Technical field
?the present invention relates to a kind of technical process and processing parameter for gas acetylene Fixed Bed Gas Phase method preparing vinyl acetate.
Background technology
Vinyl acetate between to for plastic (VAc) synthesis technique is that to take acetic acid and acetylene be raw material, take zinc acetate/gac as catalyzer, Fixed Bed Gas Phase synthesizing vinyl acetate.
Fresh acetylene enters washing tower after boosting, and acetic acid is mixed into reactor with acetylene after being heated into acetic acid steam, reacting by heating in reactor.
Prior art exists acetylene, acetic acid, and remix enters that the pressure of reactor is low after heating separately, acetylene per pass conversion is lower than 10% problem, if want, by improving acetylene intake pressure, solve the problem that acetylene per pass conversion is low, be prone to again security incident, because dry, pure acetylene is easily blasted under High Temperature High Pressure.
The object of the present invention is to provide a kind of preparation method of vinyl acetate between to for plastic, can safe and efficient raising output.
A preparation method for vinyl acetate between to for plastic, is characterized in that acetylene pressurization is rear and acetic acid Hybrid Heating, then reacts, and the pressure of described acetylene pressurization is 0.04mpa～0.07mpa, is preferably 0.048～0.07mpa, more preferably 0.07 mpa; Before pressurization, temperature is 20～30 ℃, and preferably 24～26 ℃, the temperature after pressurization is 20～60 ℃, preferably 30～50 ℃.Successfully improved the reaction system safe pressure of preparing vinyl acetate between to for plastic, the steady running of pressurizing device, both improved acetylene per pass conversion, output is significantly improved, avoid acetylene explosive under high-temperature and high-pressure conditions to produce security incident simultaneously, and the work-ing life of extension device, also avoided unstripped gas molecule to produce and freezed.
In order to improve the intermolecular compatible degree of unstripped gas and homogeneity, above-mentioned heating is divided into two stages, first stage is first acetylene and acetic acid to be mixed and heated to 110 ℃～120 ℃, be preferably 112 ℃, subordinate phase is the acetylene after first stage Hybrid Heating and acetic acid to be heated to 160～180 ℃, preferably 170 ℃.
For raw material can be reacted fully rapidly, and improve the per pass conversion of acetylene, acetylene: acetic acid is 5～12:1 as the mol ratio of raw material, is preferably 8:1.
In order to build more favourable reaction environment, the temperature of above-mentioned building-up reactions is 160 ℃～180 ℃, is preferably 170 ℃.
The production system that the preparation method of above-mentioned vinyl acetate between to for plastic uses, comprise vinyl acetate between to for plastic synthesis reactor, be connected successively with described reactor the hybrid heating device of unstripped gas, be connected with reactor refrigerating unit, acetylene pressurizing device, described acetylene pressurizing device is connected with the hybrid heating device of described unstripped gas.Acetylene and acetic acid Hybrid Heating after pressurizeing like this, thus the intake pressure that acetylene pressure improves reactor both can have been improved, can prevent that again pure, dry acetylene blast from security incident occurring.
In order further to improve the per pass conversion of acetylene, the heating unit of above-mentioned raw materials gas is comprised of the superheater communicating successively with reactor and vaporizer, and vaporizer communicates with above-mentioned acetylene pressurizing device.The staged type of heating of raw material (acetylene, acetic acid) has been improved to the dividing potential drop of acetylene, further improved the per pass conversion of acetylene.
In order to realize the recycle of acetylene, above-mentioned refrigerating unit is communicated with above-mentioned acetylene pressurizing device, between above-mentioned acetylene pressurizing device and above-mentioned raw materials gas heating unit, is also provided with washing tower.Unreacted acetylene can through pressurizeing, wash, again entering reactive system, both reduce the consumption for raw material and energy together with fresh acetylene, improved the security of system simultaneously.
In order to realize the control of maximum system energy and to utilize fully, the production system of above-mentioned vinyl acetate between to for plastic also comprises the heating plant of the described reactor consisting of hotline heater and thermal oil water cooler.Above-mentioned heating plant also comprises vapour generator, and vapour generator and thermal oil water cooler are arranged in parallel, and realize the formal transformation of energy, for the recycle of energy provides leeway more fully.
The production system of above-mentioned vinyl acetate between to for plastic, described in pass into acetylene pressurizing device be Root's blower.
The production system of above-mentioned vinyl acetate between to for plastic, described refrigerating unit is mixing condensation system, two mixing condensation towers, consists of.
beneficial effect
1.the present invention has successfully realized the optimization of vinyl acetate between to for plastic preparation flow, improving under the prerequisite of output, has also simplified Production Flow Chart, has reduced equipment and labor force's input, by input still less, brings larger benefit.
The invention solves security and the two problem that can not take into account of output of in vinyl acetate production process, existing, by optimizing, successfully improved the safe pressure of reaction system, can improve acetylene per pass conversion, make it to reach 12%～13%, output is significantly improved, avoid again acetylene explosive under high-temperature and high-pressure conditions to produce security incident.
The present invention has realized the optimization that energy utilizes, and energy is more reasonably used, and has given play to maximum effect, and falls as far as possible low-energy scattering and disappearing, thereby as reduced acetylene heating unit, reduces the loss of the energy, makes production cost reduce by 25 yuan/ton of VAC.
After acetylene per pass conversion improves, the space-time yield of reactor improves, and has improved synthetic single-row throughput, for 200,000 tons of VAC synthesizer transformations provide technical support.
Accompanying drawing explanation
The production system that Fig. 1 preparation method of the present invention adopts.
Embodiment
Further illustrate by the following examples the present invention, but the present invention is not limited to these embodiment.
embodiment 1
5 parts of fresh acetylene boost to 0.07mpa through Root's blower, and before pressurization, temperature is 20 ℃, and the temperature after pressurization is 30 ℃.Then the acetic acid that is 1 part with metering mixes, and is first heated to 115 ℃, is then heated to 160 ℃, enters reactor and carries out building-up reactions at 170 ℃, obtains vinyl acetate between to for plastic.Acetylene per pass conversion reaches 12.1%.
embodiment 2
8 parts of acetylene, comprise and the unreacted acetylene of fresh acetylene and recovery boost to 0.06mpa through Root's blower, before pressurization, temperature is 24 ℃, and the temperature after pressurization is 45 ℃.Then the acetic acid that is 1 part with metering mixes, and is first heated to 120 ℃, is then heated to 175 ℃, at 170 ℃, carries out building-up reactions, after cooling, obtains vinyl acetate between to for plastic.Reclaim unreacted acetylene, recycle.Acetylene per pass conversion is 13.2%.
embodiment 3
12 parts of acetylene, comprise and the unreacted acetylene of fresh acetylene and recovery boost to 0.05mpa through Root's blower, before pressurization, temperature is 26 ℃, and the temperature after pressurization is 50 ℃.The acetic acid that is 1 part with metering mixes, and is first heated to 110 ℃, is then heated to 180 ℃, enters reactor and carries out building-up reactions at 180 ℃, reclaims unreacted acetylene.Acetylene per pass conversion can reach 12.5%.
embodiment 4
10 parts of acetylene, comprise and the unreacted acetylene of fresh acetylene and recovery boost to 0.04mpa through Root's blower, before pressurization, temperature is 30 ℃, and the temperature after pressurization is 60 ℃.The acetic acid that is 1 part with metering mixes, and is first heated to 112 ℃, is then heated to 172 ℃, enters reactor and carries out building-up reactions at 176 ℃, obtains vinyl acetate between to for plastic.Reclaim unreacted acetylene.Acetylene per pass conversion can reach 12.3%.
Claims (10)
1. a preparation method for vinyl acetate between to for plastic, take acetic acid and acetylene as raw material, it is characterized in that acetylene pressurization is rear and acetic acid Hybrid Heating, then react, the pressure of described acetylene pressurization is 0.04mpa～0.07mpa, before pressurization, temperature is 20～30 ℃, and the temperature after pressurization is 20～60 ℃.
2. the preparation method of vinyl acetate between to for plastic as claimed in claim 1, take acetic acid and acetylene as raw material, it is characterized in that acetylene pressurization is rear and acetic acid Hybrid Heating, then react, the pressure of described acetylene pressurization is 0.048～0.07mpa, before pressurization, temperature is 24～26 ℃, and the temperature after pressurization is 30～50 ℃.
3. the preparation method of vinyl acetate between to for plastic as claimed in claim 1 or 2, described heating is divided into two stages, first stage is first by acetylene and acetic acid mixing post-heating to 110 ℃～120 ℃, and subordinate phase is that the acetylene after first stage Hybrid Heating and acetic acid are heated to 160～180 ℃.
4. the preparation method of vinyl acetate between to for plastic as claimed in claim 3, described heating is divided into two stages, and the first stage is first by acetylene and acetic acid mixing post-heating to 112 ℃, and subordinate phase is that the acetylene after first stage Hybrid Heating and acetic acid are heated to 170 ℃.
5. the preparation method of vinyl acetate between to for plastic as claimed in claim 1, acetylene: the mol ratio of acetic acid is 5～12:1.
6. the preparation method of vinyl acetate between to for plastic as claimed in claim 5, acetylene: the mol ratio of acetic acid is 8:1.
7. the preparation method of vinyl acetate between to for plastic as claimed in claim 1, synthesis reaction temperature is 160 ℃～180 ℃.
8. the production system that preparation method used of the vinyl acetate between to for plastic as described in as arbitrary in claim 1～7, comprise vinyl acetate between to for plastic synthesis reactor, be connected successively with described reactor the hybrid heating device of unstripped gas, be connected with reactor refrigerating unit, acetylene pressurizing device, described acetylene pressurizing device is connected with the hybrid heating device of described unstripped gas.
9. the production system that the preparation method of vinyl acetate between to for plastic as claimed in claim 8 uses, the heating unit of described unstripped gas is comprised of the superheater communicating successively with reactor and vaporizer, and vaporizer communicates with above-mentioned acetylene pressurizing device.
10. the production system that the preparation method of vinyl acetate between to for plastic as claimed in claim 8 uses, described refrigerating unit is communicated with described acetylene pressurizing device, between described acetylene pressurizing device and described unstripped gas heating unit, is also provided with washing tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310201504.5A CN104177258A (en) | 2013-05-27 | 2013-05-27 | Method for preparing vinyl acetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310201504.5A CN104177258A (en) | 2013-05-27 | 2013-05-27 | Method for preparing vinyl acetate |
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| CN104177258A true CN104177258A (en) | 2014-12-03 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201310201504.5A Pending CN104177258A (en) | 2013-05-27 | 2013-05-27 | Method for preparing vinyl acetate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107011163A (en) * | 2017-04-25 | 2017-08-04 | 天津大学 | The method that acetylene method gas phase produces vinylacetate |
| CN107162909A (en) * | 2017-04-25 | 2017-09-15 | 天津大学 | A kind of vinyl acetate refined thermal coupling methods and device |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA756632A (en) * | 1967-04-11 | C. Smith Leonard | Production of vinyl acetate | |
| CN85107659A (en) * | 1985-10-15 | 1987-04-15 | 沈有光 | Synthesis of vinyl acetate from acetylene by fluidized bed under pressure |
| CN101928217A (en) * | 2010-05-27 | 2010-12-29 | 国电英力特能源化工集团股份有限公司 | Novel method for synthetizing vinyl acetate by calcium carbide acetylene method |
| CN203625265U (en) * | 2013-05-27 | 2014-06-04 | 中国石油化工集团公司 | Production system of vinyl acetate |
-
2013
- 2013-05-27 CN CN201310201504.5A patent/CN104177258A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA756632A (en) * | 1967-04-11 | C. Smith Leonard | Production of vinyl acetate | |
| CN85107659A (en) * | 1985-10-15 | 1987-04-15 | 沈有光 | Synthesis of vinyl acetate from acetylene by fluidized bed under pressure |
| CN101928217A (en) * | 2010-05-27 | 2010-12-29 | 国电英力特能源化工集团股份有限公司 | Novel method for synthetizing vinyl acetate by calcium carbide acetylene method |
| CN203625265U (en) * | 2013-05-27 | 2014-06-04 | 中国石油化工集团公司 | Production system of vinyl acetate |
Non-Patent Citations (1)
| Title |
|---|
| 王勤旺: "增加电石乙炔工艺合成醋酸乙烯收率的方法", 《山西化工》, vol. 24, no. 4, 30 November 2004 (2004-11-30) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107011163A (en) * | 2017-04-25 | 2017-08-04 | 天津大学 | The method that acetylene method gas phase produces vinylacetate |
| CN107162909A (en) * | 2017-04-25 | 2017-09-15 | 天津大学 | A kind of vinyl acetate refined thermal coupling methods and device |
| CN107011163B (en) * | 2017-04-25 | 2018-05-04 | 天津大学 | The method that acetylene method gas phase produces vinylacetate |
| CN107162909B (en) * | 2017-04-25 | 2018-07-13 | 天津大学 | A kind of thermal coupling methods and device that vinyl acetate is refined |
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Application publication date: 20141203 |
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