CN108003131A - A kind of chlorocarbonic acid vinyl acetate Green production method - Google Patents

A kind of chlorocarbonic acid vinyl acetate Green production method Download PDF

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Publication number
CN108003131A
CN108003131A CN201810062774.5A CN201810062774A CN108003131A CN 108003131 A CN108003131 A CN 108003131A CN 201810062774 A CN201810062774 A CN 201810062774A CN 108003131 A CN108003131 A CN 108003131A
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China
Prior art keywords
chlorine
vinyl acetate
acid vinyl
chlorocarbonic acid
liquid
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CN201810062774.5A
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Chinese (zh)
Inventor
万保坡
吴毅杰
许金来
林刚
许智敏
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Changyuan Huasheng (taixing) Lithium Material Co Ltd
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Changyuan Huasheng (taixing) Lithium Material Co Ltd
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Application filed by Changyuan Huasheng (taixing) Lithium Material Co Ltd filed Critical Changyuan Huasheng (taixing) Lithium Material Co Ltd
Priority to CN201810062774.5A priority Critical patent/CN108003131A/en
Publication of CN108003131A publication Critical patent/CN108003131A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D317/00Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
    • C07D317/08Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
    • C07D317/10Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
    • C07D317/32Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D317/42Halogen atoms or nitro radicals

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present invention provides a kind of chlorocarbonic acid vinyl acetate Green production method, and operating procedure is as follows:1) vinylene carbonate after weighing is added in chlorination tower by head tank;2) liquid chlorine is introduced in chlorination tower;3) ultraviolet lamp is opened, by the catalytic action of ultraviolet light, chlorination reaction occurs for chlorine and ethylene carbonate in kettle, produces chlorocarbonic acid vinyl acetate;4) after reacting a period of time, chlorated liquid is gone into de- light kettle, nitrogen is passed through, the chlorine being mingled with chlorated liquid and hydrogen chloride gas is driven out of;5) chlorated liquid is transferred in tube type falling-film crystallizer, by temperature control at subzero 15 DEG C subzero 10 DEG C, gained liquid is product chlorocarbonic acid vinyl acetate.The present invention has the beneficial effect that:1) continuous production, production efficiency is high, and energy consumption is low;2) product purity is high;3) unnecessary raw material can reuse, non-environmental-pollution.

Description

A kind of chlorocarbonic acid vinyl acetate Green production method
Technical field
The present invention relates to chlorocarbonic acid ethene fat field, more particularly to a kind of chlorocarbonic acid vinyl acetate Green production method.
Background technology
Existing chlorocarbonic acid ethene fat mainly reacts generation by vinylene carbonate and chlorine under ultra violet lamp, This process reacts for intervalization in order to control by-products content, causes reaction efficiency low, product purity is low;In addition, reaction is secondary Product cannot be effectively addressed, and can cause environmental pollution.
The content of the invention
It is an object of the invention to propose a kind of chlorocarbonic acid vinyl acetate Green production method, there is production efficiency height, production The advantages that thing purity is high, non-environmental-pollution.
To achieve these goals, the present invention provides a kind of chlorocarbonic acid vinyl acetate Green production method, and operating procedure is such as Under:
1) vinylene carbonate after weighing is added in chlorination tower by head tank;
2) by liquid chlorine after chlorine liquid carburetor hot water vaporization, chlorine pressure, regulating valve control are controlled by chlorine pressure maintaining valve Preparing chlorine gas flow, is introduced in chlorination tower finally by inserting tube;
3) ultraviolet lamp is opened, by the catalytic action of ultraviolet light, chlorination reaction occurs for chlorine and ethylene carbonate in kettle, raw Produce chlorocarbonic acid vinyl acetate;
4) after reacting a period of time, chlorated liquid is gone into de- light kettle, is passed through nitrogen, by the chlorine being mingled with chlorated liquid and Hydrogen chloride gas is driven out of;
5) chlorated liquid is transferred in tube type falling-film crystallizer, by temperature control in subzero 15 DEG C -10 DEG C subzero, gained liquid Body is product chlorocarbonic acid vinyl acetate, and content 90%-95%, the vinylene carbonate solidified in crystallizer is heated and is exported To vinylene carbonate recycling kettle, recycled is into chlorination reaction.
Further, step 1) the chlorination tower tower diameter is 500-800mm, a height of 5-8m.
Further, the step 4) reaction time is 10-12h.
Further, step 4) the chlorated liquid key component content is chlorocarbonic acid vinyl acetate=50%-55%, double chlorine For ethylene carbonate=0.1%-0.5%, vinylene carbonate=45%-50%.
Further, step 5) the bottom material is mainly vinylene carbonate, its content is 85%-90%.
The present invention has the beneficial effect that:1) continuous production, production efficiency is high, and energy consumption is low;2) product purity is high;3) it is unnecessary Raw material can reuse, non-environmental-pollution.
Embodiment
The embodiment of the present invention is described below in detail.
Embodiment 1:
The present invention provides a kind of chlorocarbonic acid vinyl acetate Green production method, and operating procedure is as follows:
1) vinylene carbonate after weighing is added in chlorination tower by head tank;
2) by liquid chlorine after chlorine liquid carburetor hot water vaporization, chlorine pressure, regulating valve control are controlled by chlorine pressure maintaining valve Preparing chlorine gas flow, is introduced in chlorination tower finally by inserting tube;
3) ultraviolet lamp is opened, by the catalytic action of ultraviolet light, chlorination reaction occurs for chlorine and ethylene carbonate in kettle, raw Produce chlorocarbonic acid vinyl acetate;
4) after reacting a period of time, chlorated liquid is gone into de- light kettle, is passed through nitrogen, by the chlorine being mingled with chlorated liquid and Hydrogen chloride gas is driven out of;
5) chlorated liquid is transferred in tube type falling-film crystallizer, by temperature control at subzero 10 DEG C, gained liquid is to produce Product chlorocarbonic acid vinyl acetate, content 90.8%, the vinylene carbonate solidified in crystallizer heating is exported to carbonic acid Asia second In enester recycling kettle, recycled is into chlorination reaction.
Wherein, step 1) the chlorination tower tower diameter is 500mm, a height of 5m.
Wherein, the step 4) reaction time is 10h.
Wherein, step 4) the chlorated liquid key component content is chlorocarbonic acid vinyl acetate=51.2%, double chlorocarbonic acids Ethene fat=0.5%, vinylene carbonate=48.2%.
Wherein, step 5) the bottom material is mainly vinylene carbonate, its content is 85.8%.
Embodiment 2:
The present invention provides a kind of chlorocarbonic acid vinyl acetate Green production method, and operating procedure is as follows:
1) vinylene carbonate after weighing is added in chlorination tower by head tank;
2) by liquid chlorine after chlorine liquid carburetor hot water vaporization, chlorine pressure, regulating valve control are controlled by chlorine pressure maintaining valve Preparing chlorine gas flow, is introduced in chlorination tower finally by inserting tube;
3) ultraviolet lamp is opened, by the catalytic action of ultraviolet light, chlorination reaction occurs for chlorine and ethylene carbonate in kettle, raw Produce chlorocarbonic acid vinyl acetate;
4) after reacting a period of time, chlorated liquid is gone into de- light kettle, is passed through nitrogen, by the chlorine being mingled with chlorated liquid and Hydrogen chloride gas is driven out of;
5) chlorated liquid is transferred in tube type falling-film crystallizer, by temperature control at subzero 15 DEG C, gained liquid is to produce Product chlorocarbonic acid vinyl acetate, content 94.9%, the vinylene carbonate solidified in crystallizer heating is exported to carbonic acid Asia second In enester recycling kettle, recycled is into chlorination reaction.
Wherein, step 1) the chlorination tower tower diameter is 800mm, a height of 8m.
Wherein, the step 4) reaction time is 12h.
Wherein, step 4) the chlorated liquid key component content is chlorocarbonic acid vinyl acetate=50.1%, double chlorocarbonic acids Ethene fat=0.4%, vinylene carbonate=49.4%.
Wherein, step 5) the bottom material is mainly vinylene carbonate, its content is 89.3%.
The present invention has the beneficial effect that:1) continuous production, production efficiency is high, and energy consumption is low;2) product purity is high;3) it is unnecessary Raw material can reuse, non-environmental-pollution.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the invention, although with reference to foregoing reality Apply example the present invention is described in detail, for those skilled in the art, it still can be to foregoing each implementation Technical solution described in example is modified, or carries out equivalent substitution to which part technical characteristic.All essences in the present invention With within principle, any modification, equivalent replacement, improvement and so on, should all be included in the protection scope of the present invention god.

Claims (5)

  1. A kind of 1. chlorocarbonic acid vinyl acetate Green production method, it is characterised in that:Operating procedure is as follows:
    1) vinylene carbonate after weighing is added in chlorination tower by head tank;
    2) by liquid chlorine after chlorine liquid carburetor hot water vaporization, chlorine pressure, regulating valve control chlorine are controlled by chlorine pressure maintaining valve Throughput, is introduced in chlorination tower finally by inserting tube;
    3) ultraviolet lamp is opened, by the catalytic action of ultraviolet light, chlorination reaction occurs for chlorine and ethylene carbonate in kettle, produces chlorine For ethylene carbonate;
    4) after reacting a period of time, chlorated liquid is gone into de- light kettle, is passed through nitrogen, by the chlorine being mingled with chlorated liquid and chlorination Hydrogen is driven out of;
    5) chlorated liquid is transferred in tube type falling-film crystallizer, by temperature control subzero 15 DEG C-it is 10 DEG C subzero, gained liquid is For product chlorocarbonic acid vinyl acetate, content 90%-95%, the vinylene carbonate solidified in crystallizer heating is exported to carbon In sour vinylene recycling kettle, recycled is into chlorination reaction.
  2. A kind of 2. chlorocarbonic acid vinyl acetate Green production method according to claim 1, it is characterised in that:Step 1) the chlorine It is 500-800mm, a height of 5-8m to change tower tower diameter.
  3. A kind of 3. chlorocarbonic acid vinyl acetate Green production method according to claim 1, it is characterised in that:When step 4) is reacted Between be 10-12h.
  4. A kind of 4. chlorocarbonic acid vinyl acetate Green production method according to claim 1, it is characterised in that:Step 4) the chlorine Change liquid key component content as chlorocarbonic acid vinyl acetate=50%-55%, double chlorocarbonic acid ethene fat=0.1%-0.5%, carbon Sour vinylene=45%-50%..
  5. A kind of 5. chlorocarbonic acid vinyl acetate Green production method according to claim 1, it is characterised in that:Step 5) the kettle Bottom material is mainly vinylene carbonate, its content is 85%-90%.
CN201810062774.5A 2018-01-23 2018-01-23 A kind of chlorocarbonic acid vinyl acetate Green production method Pending CN108003131A (en)

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Application Number Priority Date Filing Date Title
CN201810062774.5A CN108003131A (en) 2018-01-23 2018-01-23 A kind of chlorocarbonic acid vinyl acetate Green production method

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CN108003131A true CN108003131A (en) 2018-05-08

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110437202A (en) * 2019-08-27 2019-11-12 许兆石 A kind of chloridization process of ethylene carbonate
CN111004203A (en) * 2020-03-11 2020-04-14 东营市海科新源化工有限责任公司 Purification method and purification device for electronic-grade ethylene carbonate
CN112979607A (en) * 2021-03-11 2021-06-18 泰兴华盛精细化工有限公司 Method for continuously preparing chlorinated ethylene carbonate
CN114437016A (en) * 2022-02-28 2022-05-06 济源市恒顺新材料有限公司 Production and manufacturing method of chlorinated ethylene carbonate
CN115677646A (en) * 2022-11-15 2023-02-03 福建致尚生物质材料发展有限公司 Method for co-producing bio-based plasticizer by using chloroethylene carbonate
CN116854658A (en) * 2023-07-11 2023-10-10 珠海光瑞新材料有限公司 Method for producing chloroethylene carbonate

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105031966A (en) * 2015-08-17 2015-11-11 天津市鹏翔科技有限公司 Multi-tube falling-film crystallizer and method
CN105503812A (en) * 2015-12-28 2016-04-20 苏州华一新能源科技有限公司 Continuous production method for high-purity vinylene carbonate
CN107540516A (en) * 2016-06-27 2018-01-05 宁夏海诚电化信息科技有限公司 A kind of chlorobenzoyl chloride prepares chloride process

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105031966A (en) * 2015-08-17 2015-11-11 天津市鹏翔科技有限公司 Multi-tube falling-film crystallizer and method
CN105503812A (en) * 2015-12-28 2016-04-20 苏州华一新能源科技有限公司 Continuous production method for high-purity vinylene carbonate
CN107540516A (en) * 2016-06-27 2018-01-05 宁夏海诚电化信息科技有限公司 A kind of chlorobenzoyl chloride prepares chloride process

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110437202A (en) * 2019-08-27 2019-11-12 许兆石 A kind of chloridization process of ethylene carbonate
CN111004203A (en) * 2020-03-11 2020-04-14 东营市海科新源化工有限责任公司 Purification method and purification device for electronic-grade ethylene carbonate
CN112979607A (en) * 2021-03-11 2021-06-18 泰兴华盛精细化工有限公司 Method for continuously preparing chlorinated ethylene carbonate
CN114437016A (en) * 2022-02-28 2022-05-06 济源市恒顺新材料有限公司 Production and manufacturing method of chlorinated ethylene carbonate
CN115677646A (en) * 2022-11-15 2023-02-03 福建致尚生物质材料发展有限公司 Method for co-producing bio-based plasticizer by using chloroethylene carbonate
CN116854658A (en) * 2023-07-11 2023-10-10 珠海光瑞新材料有限公司 Method for producing chloroethylene carbonate

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Application publication date: 20180508