CN104817097B - Recycling and reusing method of sodium bromide in synthesis process of styrene oxide - Google Patents
Recycling and reusing method of sodium bromide in synthesis process of styrene oxide Download PDFInfo
- Publication number
- CN104817097B CN104817097B CN201510221716.9A CN201510221716A CN104817097B CN 104817097 B CN104817097 B CN 104817097B CN 201510221716 A CN201510221716 A CN 201510221716A CN 104817097 B CN104817097 B CN 104817097B
- Authority
- CN
- China
- Prior art keywords
- mass parts
- sodium bromide
- temperature
- hours
- kettle
- 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.)
- Active
Links
Abstract
The invention discloses a recycling and reusing method of sodium bromide in a synthesis process of styrene oxide, which includes following steps: (1) feeding raw materials; (2) carrying out an addition reaction; (3) carrying out a saponification reaction; and (4) performing layered recycling. The recycling and reusing method is advantaged in that the sodium bromide in the synthesis process of the styrene oxide can be recycled effectively and can be used again as the raw material in the next batch of synthesis. The method can not only reduce technical cost but also greatly reduce treatment pressure and emission amount of waste water, and meanwhile can increase the yields of intermediates and products and has an excellent economic benefit.
Description
Technical field
The present invention relates to the synthesis technique of Styryl oxide, and in particular to the sodium bromide recovery side in the synthesis technique
Method.
Background technology
For a long time, in synthesizing epoxy vinylbenzene（Also known as styrene oxide）In technique, the use of sodium bromide during addition reaction
Amount is high, and in the water layer separated Jing after liquid caustic soda saponification, containing sodium bromide of the content 33% or so, if most
Eventually water layer of this part containing sodium bromide is excluded as waste water, larger pollution will be caused to environment, and makes a big purchase sodium bromide in large quantities also to want
Spend very big economic cost.Accordingly, it is desirable to provide a kind of new technical scheme is solving the above problems.
The content of the invention
The technical problem to be solved be to provide it is a kind of can effectively to the bromination in Styryl oxide synthesis technique
The method that sodium carries out recovery.
To solve above-mentioned technical problem, the technical solution used in the present invention is：
Sodium bromide recovery method, comprises the following steps in Styryl oxide synthesis technique：
（1）Feed intake：The stirring of addition kettle is opened, styrene, the 176- of 160-200 mass parts is put into successively in addition kettle
The sodium bromide of 216 mass parts and the fresh water (FW) of 430-470 mass parts；
（2）Addition reaction：Temperature in control addition kettle is added dropwise the catalyst of 210-250 mass parts, control at 45-55 DEG C
Time for adding processed is 0.8-1.2 hours, then heats to 95-100 DEG C, is incubated 1.5-2.5 hours；
（3）Saponification：After addition reaction terminates, room temperature is cooled the temperature to, and stand 0.5 hour with higher slice, then
The organic layer of 1200-1600 mass parts is taken by way of metering, instillation is furnished with the saponification kettle of 780-800 mass parts liquid caustic soda,
It is 0.8-1.4 hours to control time for adding, opens stirring, and is warming up to 45-60 DEG C, insulation 1.5-2 hours；
（4）Layering is reclaimed：After saponification terminates, 35-40 DEG C is cooled the temperature to, and stand 1 hour with higher slice, sampling
Lower aqueous layer, namely sodium bromide solution, check its density at a temperature of 25 DEG C, when density reaches 1.3-1.5 by treat down batch
Feed intake standby.
It is further preferred that above-mentioned catalyst is the concentrated sulfuric acid.
Compared with prior art, it is an advantage of the invention that：The present invention can effectively to the bromine in Styryl oxide synthesis technique
Change sodium to be reclaimed, and continue to feed intake and use in the synthesis of lower batch as raw material, both reduced process costs, and greatly subtract
Lack the processing pressure and discharge capacity of waste water, while the yield of each intermediate and product also increases, with preferable economy
Benefit.
Specific embodiment：
The present invention is described in further details with reference to embodiments, but these embodiments are not the limit to the present invention
It is fixed.
Embodiment 1
Sodium bromide recovery method, comprises the following steps in Styryl oxide synthesis technique：
（1）Feed intake：The stirring of addition kettle is opened, styrene, 176 mass parts of 160 mass parts are put into successively in addition kettle
Sodium bromide and 430 mass parts fresh water (FW)；
（2）Addition reaction：Temperature in control addition kettle is added dropwise the concentrated sulfuric acid of 210 mass parts, when control is added dropwise at 45 DEG C
Between be 0.8 hour, then heat to 95 DEG C, be incubated 1.5 hours；
（3）Saponification：After addition reaction terminates, room temperature is cooled the temperature to, and stand 0.5 little layered, then passed through
The mode of metering takes the organic layer of 1200 mass parts, and instillation is furnished with the saponification kettle of 780 mass parts liquid caustic soda, and controlling time for adding is
0.8 hour, stirring is opened, and be warming up to 45 DEG C, insulation 2 hours；
（4）Layering is reclaimed：After saponification terminates, 40 DEG C are cooled the temperature to, and stand 1 little layered, sampling lower floor water
Layer, namely sodium bromide solution checks its density for 1.42 at a temperature of 25 DEG C, meets the requirements, treat down to criticize feed intake it is standby.
Embodiment 2
Sodium bromide recovery method, comprises the following steps in Styryl oxide synthesis technique：
（1）Feed intake：The stirring of addition kettle is opened, styrene, 192 mass parts of 180 mass parts are put into successively in addition kettle
Sodium bromide and 450 mass parts fresh water (FW)；
（2）Addition reaction：Temperature in control addition kettle is added dropwise the concentrated sulfuric acid of 230 mass parts, when control is added dropwise at 50 DEG C
Between be 1 hour, then heat to 98 DEG C, be incubated 2 hours；
（3）Saponification：After addition reaction terminates, room temperature is cooled the temperature to, and stand 1 little layered, then by meter
The mode of amount takes the organic layer of 1400 mass parts, and instillation is furnished with the saponification kettle of 790 mass parts liquid caustic soda, and controlling time for adding is
1.2 hours, stirring is opened, and be warming up to 50 DEG C, insulation 1.8 hours；
（4）Layering is reclaimed：After saponification terminates, 37 DEG C are cooled the temperature to, and stand 3 little layereds, take lower aqueous layer
Sample, checks its density for 1.42 at a temperature of 25 DEG C, meets the requirements, treat down to criticize feed intake it is standby.
Embodiment 3
Sodium bromide recovery method, comprises the following steps in Styryl oxide synthesis technique：
（1）Feed intake：The stirring of addition kettle is opened, styrene, 216 mass parts of 200 mass parts are put into successively in addition kettle
Sodium bromide and 470 mass parts fresh water (FW)；
（2）Addition reaction：Temperature in control addition kettle is added dropwise the concentrated sulfuric acid of 250 mass parts, when control is added dropwise at 55 DEG C
Between be 1.2 hours, then heat to 100 DEG C, be incubated 2.5 hours；
（3）Saponification：After addition reaction terminates, room temperature is cooled the temperature to, and stand 1.5 little layereds, then passed through
The mode of metering takes the organic layer of 1600 mass parts, and instillation is furnished with the saponification kettle of 800 mass parts liquid caustic soda, and controlling time for adding is
1.4 hours, stirring is opened, and be warming up to 60 DEG C, insulation 1.5 hours；
（4）Layering is reclaimed：After saponification terminates, 35 DEG C are cooled the temperature to, and stand 5 little layereds, take lower aqueous layer
Sample, checks its density for 1.43 at a temperature of 25 DEG C, meets the requirements, treat down to criticize feed intake it is standby.
Claims (1)
1. sodium bromide recovery method in Styryl oxide synthesis technique, it is characterised in that comprise the following steps：
（1）Feed intake：The stirring of addition kettle is opened, styrene, the 176-216 matter of 160-200 mass parts is put into successively in addition kettle
The sodium bromide of amount part and the fresh water (FW) of 430-470 mass parts；
（2）Addition reaction：Temperature in control addition kettle is added dropwise the catalyst of 210-250 mass parts, control drop at 45-55 DEG C
Plus the time is 0.8-1.2 hours, 95-100 DEG C is then heated to, be incubated 1.5-2.5 hours；The catalyst is the concentrated sulfuric acid；
（3）Saponification：After addition reaction terminates, room temperature is cooled the temperature to, and stand 0.5 hour with higher slice, then passed through
The mode of metering takes the organic layer of 1200-1600 mass parts, and instillation is furnished with the saponification kettle of 780-800 mass parts liquid caustic soda, is controlled
Time for adding is 0.8-1.4 hours, opens stirring, and is warming up to 45-60 DEG C, insulation 1.5-2 hours；
（4）Layering is reclaimed：After saponification terminates, 35-40 DEG C is cooled the temperature to, and stand 1 hour with higher slice, sample lower floor
Water layer, namely sodium bromide solution, check its density at a temperature of 25 DEG C, when density reaches 1.3-1.5 by treat down batch to feed intake
It is standby.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510221716.9A CN104817097B (en) | 2015-05-05 | 2015-05-05 | Recycling and reusing method of sodium bromide in synthesis process of styrene oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510221716.9A CN104817097B (en) | 2015-05-05 | 2015-05-05 | Recycling and reusing method of sodium bromide in synthesis process of styrene oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104817097A CN104817097A (en) | 2015-08-05 |
| CN104817097B true CN104817097B (en) | 2017-05-10 |
Family
ID=53727609
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510221716.9A Active CN104817097B (en) | 2015-05-05 | 2015-05-05 | Recycling and reusing method of sodium bromide in synthesis process of styrene oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104817097B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109987787A (en) * | 2019-03-05 | 2019-07-09 | 天津大学 | A kind of processing method of high organic wastewater with high salt |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4894467A (en) * | 1986-10-16 | 1990-01-16 | The Standard Oil Company | Vapor phase oxidation or styrene to styrene oxide |
| CN101972665A (en) * | 2010-10-26 | 2011-02-16 | 中国科学院山西煤炭化学研究所 | Styrene epoxidizing catalyst as well as preparation method and application thereof |
| CN102311408A (en) * | 2010-06-30 | 2012-01-11 | 山东瀛洋香精香料有限公司 | Method for preparing styrene oxide by waste water zero discharge process |
| CN103204830A (en) * | 2012-01-13 | 2013-07-17 | 中国石油化工股份有限公司 | Catalytic oxidation method of styrene |
| CN103788023A (en) * | 2012-10-31 | 2014-05-14 | 中国科学院大连化学物理研究所 | Method for preparing styrene oxide through epoxidation of styrene |
-
2015
- 2015-05-05 CN CN201510221716.9A patent/CN104817097B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4894467A (en) * | 1986-10-16 | 1990-01-16 | The Standard Oil Company | Vapor phase oxidation or styrene to styrene oxide |
| CN102311408A (en) * | 2010-06-30 | 2012-01-11 | 山东瀛洋香精香料有限公司 | Method for preparing styrene oxide by waste water zero discharge process |
| CN101972665A (en) * | 2010-10-26 | 2011-02-16 | 中国科学院山西煤炭化学研究所 | Styrene epoxidizing catalyst as well as preparation method and application thereof |
| CN103204830A (en) * | 2012-01-13 | 2013-07-17 | 中国石油化工股份有限公司 | Catalytic oxidation method of styrene |
| CN103788023A (en) * | 2012-10-31 | 2014-05-14 | 中国科学院大连化学物理研究所 | Method for preparing styrene oxide through epoxidation of styrene |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104817097A (en) | 2015-08-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101250113B (en) | Method for refining p-phenylene diamine | |
| CN101659606A (en) | Method for producing calcium formate by using industrial waste liquid | |
| CN106496039B (en) | The separation method of nitrochlorobenzene meta-position oil intermediate nitro Benzene Chloride and para-nitrochloro-benzene, ortho-nitrochlorobenzene | |
| CN106632080A (en) | Flucytosine manufacturing process | |
| CN104817097B (en) | Recycling and reusing method of sodium bromide in synthesis process of styrene oxide | |
| CN107793328A (en) | A kind of production method of N, N cyanoethyl benzylaniline | |
| CN105503582A (en) | Continuous production method for trifluoro monochloro chrysanthemic acid | |
| CN103951557B (en) | A kind of method with inorganic base for catalyst preparing fenofibrate | |
| CN102827041A (en) | Preparation method of p-methylsulfurylbenzaldehyde | |
| CN107083490A (en) | A kind of organic silicon chemical waste residue processing method | |
| CN104844444B (en) | Unilateral line is thermally integrated the method that azeotropic distillation extracts acetic acid in saliferous aqueous acetic acid | |
| CN107253916B (en) | A kind of environmentally protective new method for preparing amion acetic acid | |
| CN106349086A (en) | Method for preparing p-phenylenediamine rubber aging inhibitor | |
| CN102992949B (en) | Industrialized recycling method for o-chlorobenzaldehyde residual liquor | |
| CN102898321A (en) | Method for preparing N-butoxy oxalyl butyl alaninate | |
| CN101979380A (en) | Method for synthesizing 3-methylpyridine | |
| CN105367415B (en) | A kind of waste PET materials chemistry method reclaims circulation recycling system | |
| CN111533683B (en) | Method and device for preparing vinyl pyridine by continuous dehydration of hydroxyethyl pyridine | |
| CN104341337B (en) | A kind of discoloration method of pyridiniujm finished product | |
| CN106986762A (en) | A kind of technique for preparing DL mandelic acids | |
| CN106632062A (en) | Preparation method of tinidazole | |
| CN106397469A (en) | Continuous cycle preparation method of trimethyl borate | |
| CN1026181C (en) | Cracking of disgenin and new art of mother liquor recovery therefrom | |
| CN104058442A (en) | Processing process for heating aluminum fluoride step by step | |
| CN106554267A (en) | The method for improving gallic acid extraction ratio |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201027 Address after: No.18, Jinlong Road, Chunjiang Town, Xinbei District, Changzhou City, Jiangsu Province, 213000 Patentee after: CHANGZHOU YABANG-QH PHARMACHEM Co.,Ltd. Patentee after: Inner Mongolia Qihui Pharmaceutical Co., Ltd Patentee after: LIANYUNGANG YAHUI PHARMACHEM Co.,Ltd. Address before: 226100, Jiangsu, Nantong Haimen Ling industrial concentration zone Patentee before: NANTONG HAISHENG PHARMACEUTICAL Co.,Ltd. |