CN105859509B - A kind of chloropropene purification process and its application - Google Patents
A kind of chloropropene purification process and its application Download PDFInfo
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- CN105859509B CN105859509B CN201610230379.4A CN201610230379A CN105859509B CN 105859509 B CN105859509 B CN 105859509B CN 201610230379 A CN201610230379 A CN 201610230379A CN 105859509 B CN105859509 B CN 105859509B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/389—Separation; Purification; Stabilisation; Use of additives by adsorption on solids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/395—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to a chemical modification of at least one compound
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of chloropropene purification process and its application, purification process to include the following steps：Chloropropene is dried with drier first, the chloropropene after drying is purified again with solid state reduction agent, and chloropropene after purification carries out final purification with alkaline matter again.Using the chloropropene water white transparency of this method after purification, purity reaches 99.5wt% or more, and property indices reach requirement.The raw material that purification process uses is cheap and easily-available, reduces the cost of chloropropene purifying, and each process carries out under mild conditions, need not provide extraneous energy, energy conservation and environmental protection.The method of the present invention is simple and practicable, not dangerous.
Description
Technical field
The present invention relates to a kind of chloropropene purification process and its applications.
Background technology
Chloropropene, chemicals, colourless liquid are a kind of important organic synthesis raw materials.Particularly, chloropropene is synthesis 1-
One of two kinds of raw materials of allyl -3- methylimidazole villaumite ionic liquids, and the latter is the direct solvent of cellulose, can be used extensively
In preparing the regenerated cellulose products such as fiber, film.However chloropropene stability is poor, and storing and be easy to inhale in transportational process
Aqueous metamorphism, and hydrogen chloride is decomposited, not only make the reduction of its purity, but also discoloration of turning to be yellow, and then influence to use.Therefore, by chlorine
Propylene is as raw material for before synthetic reaction, it is necessary to chloropropene be carried out purification process, improves chloropropene purity, otherwise impurity
In the presence of can not only increase side reaction, the purity of product is reduced, improves the difficulty and cost of product purification, but also is likely to result in
Catalyst failure causes reaction to fail, or generates dangerous.And there is presently no the preferable methods purified to chloropropene.
Invention content
In order to overcome the above-mentioned deficiencies of the prior art, the present invention provides a kind of chloropropene purification process and its applications.It should
Method can preferably purify chloropropene, improve the quality of chloropropene.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of chloropropene purification process, includes the following steps：Chloropropene is dried with drier first, after dry
Chloropropene is purified again with solid state reduction agent, and chloropropene after purification carries out final purification with alkaline matter again, obtains
The chloropropene of high-purity.
This is sequentially specific, and final purification process can remove the acidic materials of first two steps purification step generation, is protected
Card impurity most effectively removes, and then ensure that the purification effect of chloropropene.
Preferably, every 100 parts of chloropropenes are purified using 0.5-5.0 parts of drier.Drier is act as except dechlorination
Water in propylene.
Preferably, the drier is anhydrous calcium chloride, anhydrous magnesium sulfate, anhydrous sodium sulfate, calcium oxide, calcium hydride, five
Aoxidize two phosphorus, molecular sieve or silica gel.
Preferably, dry temperature is 0-35 DEG C, and the dry time is 0.5-3h.
Chloropropene after preliminary purification is purified chloropropene fraction collection by distillation again.Stirring can promote
The mixing of chloropropene and drier, and then accelerate water removal rate and save the time under the premise of improving purification effect.
Preferably, again in purification process, the addition of solid state reduction agent is the 0.1-1.0% of chloropropene quality.
Solid state reduction agent can be reacted with the oxidative impurities in chloropropene, and then obtain the even colourless chlorine third of low coloration
Alkene.
It is further preferred that solid state reduction agent is frerrous chloride, dinitrophenylhydrazine, ascorbic acid or vitamin C.
It is further preferred that the temperature purified again is 0-35 DEG C, time 2-3h.
Chloropropene fraction collection is carried out final purification by chloropropene after purification by distillation again.Stirring can promote
The mixing of chloropropene and solid state reduction agent, and then accelerate impurity removal rate, under the premise of improving purification effect, when saving
Between.
Preferably, during final purification, alkaline matter addition is the 0.5-5% of chloropropene quality.Alkaline matter can
To be reacted with the acid impurities in chloropropene, and then remove the acid impurities in chloropropene.
It is further preferred that alkaline matter is potassium hydroxide, sodium hydroxide, sodium oxide molybdena, calcium oxide, sodium bicarbonate, carbonic acid
Sodium.
Still more preferably, the temperature of final purification is 20-35 DEG C, time 2-3h.
Still more preferably, final purification process carries out under stirring.Chloropropene after purification is by steaming
It evaporates, fraction is collected to obtain the chloropropene of high-purity.
The invention further relates to application of the above-mentioned chloropropene purification process in chlorohydrocarbon purifying, especially in chloropropene purifying
Application.
The present invention advantageous effects be：
1, the chloropropene water white transparency using this method after purification, purity reach 99.5wt% or more, are suitble to chloropropene
For the requirement of the chemical reaction of raw material, the purity and presentation quality of reaction product are improved.
2, the raw material that method of the invention uses is cheap and easily-available, reduces the cost of chloropropene purifying, and it is each during
It carries out under mild conditions, extraneous energy, energy conservation and environmental protection need not be provided.
3, method of the invention is simple and practicable, not dangerous.
Specific implementation mode
The present invention is further explained in the light of specific embodiments.
Embodiment 1
A kind of chloropropene purification process, includes the following steps：100 parts of chloropropenes are mixed with 1 part of anhydrous calcium chloride first,
Preliminary purification is carried out, the temperature of purifying is 25 DEG C, time 30min；Chloropropene fraction is collected by distillation after preliminary purification,
0.1 portion of dinitrophenylhydrazine is added in 100 parts of fractions to be purified again, the temperature purified again is 25 DEG C, time 2h；Again
Chloropropene fraction is collected by distillation after purification, 2 parts of calcium oxide are added in 100 parts of fractions and carry out final purification, the temperature of purifying
Degree is 25 DEG C, time 2h；Fraction is collected to obtain the chloropropene of high-purity by chloropropene after purification by distillation.Three
A purification process is stirred, and improves purification efficiency.
Chloropropene water white transparency after purification, purity reach 99.7wt%, and it is original that property indices, which reach with chloropropene,
The requirement of the chemical reaction of material.
Embodiment 2
A kind of chloropropene purification process, includes the following steps：100 parts of chloropropenes are mixed with 2 parts of phosphorus pentoxides first,
Preliminary purification is carried out, the temperature of purifying is 30 DEG C, time 50min；Chloropropene fraction is collected by distillation after preliminary purification,
1 part of ascorbic acid is added in 100 parts of fractions to be purified again, the temperature purified again is 30 DEG C, time 3h；It purifies again
Chloropropene fraction is collected by distillation afterwards, 5 parts of sodium bicarbonates are added in 100 parts of fractions and carry out final purification, the temperature of purifying
It is 30 DEG C, time 3h；Fraction is collected to obtain the chloropropene of high-purity by chloropropene after purification by distillation.Three
Purification process is stirred, and improves purification efficiency.
Chloropropene water white transparency after purification, purity reach 99.9wt%, and it is original that property indices, which reach with chloropropene,
The requirement of the chemical reaction of material.
Embodiment 3
A kind of chloropropene purification process, includes the following steps：100 parts of chloropropenes are mixed with 0.5 part of calcium hydride first, into
The temperature of row preliminary purification, purifying is 35 DEG C, time 60min；Chloropropene fraction is collected by distillation after preliminary purification,
0.5 part of frerrous chloride is added in 100 parts of fractions to be purified again, the temperature purified again is 35 DEG C, time 2.5h；Again
Chloropropene fraction is collected by distillation after purification, 3 parts of sodium carbonate are added in 100 parts of fractions and carry out final purification, the temperature of purifying
Degree is 35 DEG C, time 2.5h；Fraction is collected to obtain the chloropropene of high-purity by chloropropene after purification by distillation.
Three purification process are stirred, and improve purification efficiency.
Chloropropene water white transparency after purification, purity reach 99.8wt%, and it is original that property indices, which reach with chloropropene,
The requirement of the chemical reaction of material.
Embodiment 4
A kind of chloropropene purification process, includes the following steps：100 parts of chloropropenes are mixed with 5 parts of molecular sieves first, are carried out
The temperature of preliminary purification, purifying is 0 DEG C, time 3h；Chloropropene fraction is collected by distillation after preliminary purification, is evaporated at 100 parts
0.5 part of vitamin C is added in point to be purified again, the temperature purified again is 0 DEG C, time 2h；Pass through after purification again
Chloropropene fraction is collected in distillation, and 0.5 part of sodium oxide molybdena is added in 100 parts of fractions and carries out final purification, and the temperature of purifying is 20 DEG C,
Time is 2h；Fraction is collected to obtain the chloropropene of high-purity by chloropropene after purification by distillation.Three purification process
It is stirred, improves purification efficiency.
Chloropropene water white transparency after purification, purity reach 99.5wt%, and it is original that property indices, which reach with chloropropene,
The requirement of the chemical reaction of material.
Although the above-mentioned specific implementation mode to the present invention is described, the limitation not to invention protection domain,
Those skilled in the art should understand that based on the technical solutions of the present invention, those skilled in the art need not pay
The various modifications or changes that creative work can be made are still within the scope of the present invention.
Claims (7)
1. a kind of chloropropene purification process, it is characterised in that：Include the following steps：Chloropropene is done with drier first
Dry, the chloropropene after drying is purified again with solid state reduction agent, and chloropropene after purification is carried out most with alkaline matter again
After purify, obtain the chloropropene of high-purity；
Every 100 parts of chloropropenes are purified using 0.5-5.0 parts of drier；
The drier is anhydrous calcium chloride, anhydrous magnesium sulfate, anhydrous sodium sulfate, calcium oxide, calcium hydride, phosphorus pentoxide, divides
Son sieve or silica gel；
Again in purification process, the addition of solid state reduction agent is the 0.1-1.0% of chloropropene quality；
Solid state reduction agent is frerrous chloride, dinitrophenylhydrazine, ascorbic acid or vitamin C；
During final purification, the amount that alkaline matter is added is the 0.5-5% of chloropropene quality.
2. chloropropene purification process according to claim 1, it is characterised in that：Dry temperature is 0-35 DEG C, dry
Time is 0.5-3h.
3. chloropropene purification process according to claim 1, it is characterised in that：The temperature purified again is 0-35 DEG C, when
Between be 2-3h.
4. chloropropene purification process according to claim 1, it is characterised in that：Alkaline matter is potassium hydroxide, hydroxide
Sodium, sodium oxide molybdena, calcium oxide, sodium bicarbonate, sodium carbonate.
5. chloropropene purification process according to claim 1, it is characterised in that：The temperature of final purification process is 20-35
DEG C, time 2-3h.
6. chloropropene purification process according to claim 1, it is characterised in that：Three purification process are under stirring
It carries out.
7. application of any chloropropene purification process of claim 1-6 in chlorohydrocarbon purifying.
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| CN109867585A (en) * | 2017-12-01 | 2019-06-11 | 中国科学院大连化学物理研究所 | A kind of chloropropene prepares epichlorohydrin reaction process waste gas processing method |
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| CN1163461C (en) * | 2000-10-20 | 2004-08-25 | 中国石化集团巴陵石油化工有限责任公司 | Method of solving the problem of storage discolor of 3-chloro-propene |
| CN1120147C (en) * | 2001-04-10 | 2003-09-03 | 中国石化集团巴陵石油化工有限责任公司 | Method for inhibiting and eliminating discolouration of 3-chloropropene product |
| CN1307136C (en) * | 2004-08-24 | 2007-03-28 | 中国石化集团巴陵石油化工有限责任公司 | Method of preventing and eliminating discolor of 3-chloropropylene |
| CN101092327A (en) * | 2006-06-20 | 2007-12-26 | 中国石化集团巴陵石油化工有限责任公司 | Method for achromatizing 3 - allyl chloride |
| CN104557445A (en) * | 2013-10-22 | 2015-04-29 | 中国石油化工股份有限公司 | Method for decoloring chloropropene and preventing chloropropene from discoloring in storage process |
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Inventor after: Zhang Jun Inventor after: Zhang Xiaoyu Inventor after: Yu Jian Inventor after: Xue Yu Inventor after: Wu Jin Inventor after: Xu Lili Inventor after: Zhang Jinming Inventor after: Jia Fengwei Inventor before: Zhang Jun Inventor before: Zhang Xiaoyu Inventor before: Wu Jin Inventor before: Xue Yu Inventor before: Yu Jian Inventor before: Xu Lili Inventor before: Zhang Jinming Inventor before: Jia Fengwei |
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Effective date of registration: 20171212 Address after: 100190 Haidian District, Zhongguancun, North Street, No. 1, No. 2, Beijing Applicant after: Institute of Chemistry, Chinese Academy of Sciences Applicant after: Bian Shoujuan Applicant after: SHANDONG HENGLIAN NEW MATERIALS CO., LTD. Applicant after: Zhang Xiaoyu Applicant after: Xu Lili Applicant after: Jia Fengwei Applicant after: Zhang Dongguang Applicant after: Cui Zengliang Applicant after: Xian Bingbin Applicant after: Li Junbo Address before: 100190 Haidian District, Zhongguancun, North Street, No. 1, No. 2, Beijing Applicant before: Institute of Chemistry, Chinese Academy of Sciences Applicant before: SHANDONG HENGLIAN NEW MATERIALS CO., LTD. |
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Effective date of registration: 20180913 Address after: 261106 Hanting District, Weifang, Shandong Province solid embankment street office Lingang Industrial Park North District Patentee after: Shandong Zhongke Heng Lian biological base material Co., Ltd. Address before: 100190 north one street, Zhongguancun, Haidian District, Beijing, No. 2 Co-patentee before: Shandong Henglian New Material Co., Ltd. Patentee before: Institute of Chemistry, Chinese Academy of Sciences Co-patentee before: Zhang Xiaoyu Co-patentee before: Xu Lili Co-patentee before: Jia Fengwei Co-patentee before: Zhang Dongguang Co-patentee before: Cui Zengliang Co-patentee before: Xian Bingbin Co-patentee before: Li Junbo Co-patentee before: Bian Shoujuan |
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