CN109503306A - A kind of polymerization inhibitors for styrene rectification and its production method - Google Patents

A kind of polymerization inhibitors for styrene rectification and its production method Download PDF

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Publication number
CN109503306A
CN109503306A CN201910011402.4A CN201910011402A CN109503306A CN 109503306 A CN109503306 A CN 109503306A CN 201910011402 A CN201910011402 A CN 201910011402A CN 109503306 A CN109503306 A CN 109503306A
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styrene
polymerization inhibitors
polyacrylamide
polymerization
nano silica
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CN109503306B (en
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范啸
范毅
樊纪利
张洁
邵至央
缪淼
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Anhui Zhuo Yuan Chemical Technology Co Ltd
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Anhui Zhuo Yuan Chemical Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/04Purification; Separation; Use of additives by distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/20Use of additives, e.g. for stabilisation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Water Supply & Treatment (AREA)
  • Polymerisation Methods In General (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a kind of polymerization inhibitors for styrene rectification and its production methods, the polymerization inhibitors for styrene rectification is made of by weight percentage following components: di-tert- butyl nitroxide 25-55%, ethyl alcohol 10-15%, compound water soluble dispersing agent 3-8%, nano silica loads polyacrylamide 0.5-1%, water surplus.Polymerization inhibitors for styrene rectification of the invention can effectively inhibit the polymerization reaction of styrene, the catalytic activity of iron ion can be reduced again, to reduce the external inducement that styrene monomer generates polymerization from source, and it is peace and quiet to aggregated part dispersion, polymerization inhibition effect is improved through a variety of ways, substantially increases the operation stability of distillation system.

Description

A kind of polymerization inhibitors for styrene rectification and its production method
Technical field
The present invention relates to technical field of petrochemical industry more particularly to a kind of polymerization inhibitors for styrene rectification and its production method.
Background technique
Styrene is a kind of important basic organic chemical industry raw material, is industrially mainly used for the synthesis such as polystyrene, SBS The production of resin, ion exchange resin and synthetic rubber etc., application are very extensive.Currently, the production of styrene mainly uses Ethylbenzene dehydrogenation technique is divided into hydrocarbonylation workshop section, ethylbenzene rectification section, ethylbenzene dehydrogenation workshop section and phenyl ethylene rectification workshop section.
Styrene monomer has autohemagglutination property, can occur polymerize under room temperature, temperature is higher, and polymerization speed is got over Fastly.Due in the dehydrogenation reaction liquid of ethylbenzene dehydrogenation workshop section with the presence of a small amount of impurity, it is therefore desirable to pass through subsequent styrene rectifying Workshop section's processing.In distillation process, styrene monomer is easy to happen polymerization, not only influences normal production, but also increase energy consumption, Even large area is caused to stop production when serious.In order to reduce the polymerization losses of styrene monomer in distillation process, guarantee distillation system It operates normally, it is necessary to the polymerization inhibitor for inhibiting styrene polymerization be added in distillation process.
Styrene is polymerized to free radical polymerization, and influence factor includes monomer concentration, system temperature, impurity etc..Existing benzene The formula of ethylene distillation polymerization inhibitor is that single di-tert- butyl nitroxide (DTBNO) is dissolved in water in proportion, the recipe ingredient And performance is single, can not reduce the external inducement that styrene monomer generates polymerization, control polymerization effect is limited, it is necessary to It is made improvements.
Summary of the invention
The object of the invention is to remedy the disadvantages of known techniques, provides a kind of polymerization inhibitors for styrene rectification and its production Method, the polymerization inhibitors for styrene rectification can effectively inhibit the polymerization reaction of styrene and reduce the catalytic activity of iron ion, To reduce the external inducement that styrene monomer generates polymerization from source, and aggregated part is dispersed clear Only, polymerization inhibition effect is improved through a variety of ways, is conducive to the operation stability for improving distillation system.
The present invention is achieved by the following technical solutions:
A kind of polymerization inhibitors for styrene rectification is made of by weight percentage following components: di-tert- butyl nitroxide 25- 55%, ethyl alcohol 10-15%, compound water soluble dispersing agent 3-8%, nano silica load polyacrylamide 0.5-1%, more than water Amount.
The compound water soluble dispersing agent is by alkali modification sodium lignin sulfonate 30D, sapn S-40, anionic surfactant AEO-9 is by weight (3-5): (1-2): (1-2) is mixed.
Nano silica load polyacrylamide the preparation method is as follows: nano silica is added to the water point The nano silica suspension for uniformly obtaining that solid content is 1-1.5% is dissipated, it is the poly- of 0.5-1% that appropriate mass fraction, which is then added, Acrylamide aqueous solution stirs 12-24h, and nano silica load polyacrylamide is obtained after centrifugation, drying.
The volume ratio of the nano silica suspension and polyacrylamide solution is 1:(0.5-1).
The production method of the polymerization inhibitors for styrene rectification includes the following steps:
(1) compound water soluble dispersing agent, nano silica load polyacrylamide are added to the water and are dispersed with stirring uniformly, Obtain mixed liquor;
(2) di-tert- butyl nitroxide is added in ethyl alcohol, is then uniformly mixed, is filtered to remove miscellaneous with the mixed liquor Matter to get.
The invention has the advantages that
The present invention is on the basis of the formula of common styrene rectifying polymerization inhibitor, by adding by alkali modification sodium lignin sulfonate The compound water soluble dispersing agent that 30D, sapn S-40, anionic surfactant AEO-9 are formed, can be under the high temperature conditions to The good peace and quiet effect of dispersion is played in aggregated part, keeps the good clean conditions of phenyl ethylene rectification process;Pass through addition Nano silica loads polyacrylamide, iron ion can be complexed, and iron ion catalytic activity is reduced, to alleviate iron The catalytic polymerization that ion participates in.By the compound synergic of above-mentioned raw materials, there is the polymerization inhibitors for styrene rectification of production can Effect inhibits the polymerization reaction of styrene, and can reduce the catalytic activity of iron ion, produces to reduce styrene monomer from source The external inducement of raw polymerization, and it is peace and quiet to aggregated part dispersion, polymerization inhibition effect is improved through a variety of ways, greatly The operation stability of distillation system is improved greatly.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to Limit the present invention.
A kind of polymerization inhibitors for styrene rectification is made of: di-tert- butyl nitroxide by weight percentage following components 25%, ethyl alcohol 10%, compound water soluble dispersing agent 3%, nano silica load polyacrylamide 0.5%, water surplus.
The compound water soluble dispersing agent is by alkali modification sodium lignin sulfonate 30D, sapn S-40, anionic surfactant AEO-9 is mixed by weight 3:1:1.
Nano silica load polyacrylamide the preparation method is as follows: nano silica is added to the water point It dissipates and uniformly obtains the nano silica suspension that solid content is 1%, the polyacrylamide that appropriate mass fraction is 0.5% is then added Amine aqueous solution stirs 12h, and nano silica load polyacrylamide is obtained after centrifugation, drying.
The volume ratio of the nano silica suspension and polyacrylamide solution is 1:0.5.
The production method of the polymerization inhibitors for styrene rectification includes the following steps:
(1) compound water soluble dispersing agent, nano silica load polyacrylamide are added to the water and are dispersed with stirring uniformly, Obtain mixed liquor;
(2) di-tert- butyl nitroxide is added in ethyl alcohol, is then uniformly mixed, is filtered to remove miscellaneous with the mixed liquor Matter to get.
It takes the above-mentioned polymerization inhibitor of 100ppm that 110 DEG C of oil bath processing 2h in 100g styrene are added to be dried with ethanol elution polymer Polymer weight is weighed after dry, obtaining polymer weight is 0.3g.

Claims (5)

1. a kind of polymerization inhibitors for styrene rectification, which is characterized in that the polymerization inhibitors for styrene rectification is by following components by weight hundred Divide than composition: di-tert- butyl nitroxide 25-55%, ethyl alcohol 10-15%, compound water soluble dispersing agent 3-8%, nano-silica SiClx loads polyacrylamide 0.5-1%, water surplus.
2. a kind of polymerization inhibitors for styrene rectification according to claim 1, which is characterized in that the compound water soluble dispersing agent By alkali modification sodium lignin sulfonate 30D, sapn S-40, anionic surfactant AEO-9 by weight (3-5): (1-2): (1- 2) it mixes.
3. a kind of polymerization inhibitors for styrene rectification according to claim 1, which is characterized in that the nano silica load Polyacrylamide is uniformly dispersed to obtain solid content the preparation method is as follows: nano silica is added to the water as 1-1.5%'s Then nano silica suspension is added the polyacrylamide solution that appropriate mass fraction is 0.5-1% and stirs 12-24h, from Nano silica load polyacrylamide is obtained after the heart, drying.
4. a kind of polymerization inhibitors for styrene rectification according to claim 3, which is characterized in that the nano silica suspension Volume ratio with polyacrylamide solution is 1:(0.5-1).
5. a kind of production method of polymerization inhibitors for styrene rectification according to claim 1, which is characterized in that including walking as follows It is rapid:
(1) compound water soluble dispersing agent, nano silica load polyacrylamide are added to the water and are dispersed with stirring uniformly, obtained Mixed liquor;
(2) di-tert- butyl nitroxide is added in ethyl alcohol, is then uniformly mixed with the mixed liquor, is filtered to remove impurity, To obtain the final product.
CN201910011402.4A 2019-01-07 2019-01-07 Styrene rectification polymerization inhibitor and production method thereof Active CN109503306B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110330404A (en) * 2019-07-02 2019-10-15 宜兴市中大凯水处理有限公司 A kind of polymerization inhibitors for styrene rectification and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103467230A (en) * 2013-07-24 2013-12-25 金浦新材料股份有限公司 Water-soluble styrene polymerization inhibitor
CN104447182A (en) * 2014-12-05 2015-03-25 天津科技大学 Magnetically-separable solid polymerization inhibitor as well as preparation method and application thereof
US20150152053A1 (en) * 2013-12-03 2015-06-04 Ecolab USA, Inc. Nitroxide hydroxylamine and phenylenediamine combinations as polymerization inhibitors for ethylenically unsaturated monomer processes
CN108341737A (en) * 2017-01-23 2018-07-31 中国石油化工股份有限公司 The rectifying polymerization inhibitor of aromatic olefin monomers, preparation method and applications method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103467230A (en) * 2013-07-24 2013-12-25 金浦新材料股份有限公司 Water-soluble styrene polymerization inhibitor
US20150152053A1 (en) * 2013-12-03 2015-06-04 Ecolab USA, Inc. Nitroxide hydroxylamine and phenylenediamine combinations as polymerization inhibitors for ethylenically unsaturated monomer processes
CN104447182A (en) * 2014-12-05 2015-03-25 天津科技大学 Magnetically-separable solid polymerization inhibitor as well as preparation method and application thereof
CN108341737A (en) * 2017-01-23 2018-07-31 中国石油化工股份有限公司 The rectifying polymerization inhibitor of aromatic olefin monomers, preparation method and applications method

Non-Patent Citations (1)

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Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110330404A (en) * 2019-07-02 2019-10-15 宜兴市中大凯水处理有限公司 A kind of polymerization inhibitors for styrene rectification and preparation method thereof

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