CN106986771A - A kind of method of continuous production DMSS - Google Patents
A kind of method of continuous production DMSS Download PDFInfo
- Publication number
- CN106986771A CN106986771A CN201710409685.9A CN201710409685A CN106986771A CN 106986771 A CN106986771 A CN 106986771A CN 201710409685 A CN201710409685 A CN 201710409685A CN 106986771 A CN106986771 A CN 106986771A
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- CN
- China
- Prior art keywords
- dmss
- dimethyl succinate
- continuous production
- continuous
- added dropwise
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
- C07C67/313—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by introduction of doubly bound oxygen containing functional groups, e.g. carboxyl groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
- C07C67/333—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by isomerisation; by change of size of the carbon skeleton
- C07C67/343—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms
Abstract
The invention provides a kind of method of continuous production DMSS, the technical scheme performs Claisen condensation reaction and the Michael Diekmann condensation reaction of dimethyl succinate and sodium methoxide in the way of being continuously added dropwise, continuous discharging can be realized, collect and be acidified again by dilute sulfuric acid after certain product, obtain DMSS.The present invention is based on Classic Experiments principle design, the improvement of mode of operation forms brand-new technical process, and the technical scheme shortens the reaction time, while reducing energy consumption, so that production efficiency is obviously improved, while overcoming the problem of quality discrepancy is larger between different batches in batch production mode.The present invention realizes good technique effect with innovative technological improvement, while cost is relatively low, be easily achieved, therefore with good promotion prospect.
Description
Technical field
The present invention relates to chemical production technical field, further to the synthetic method of fuel intermediate, and in particular to one
The method for planting continuous production DMSS.
Background technology
DMSS is the synthesis most representative key intermediate of quinacridone-type pigments, for producing
The DMSS of quinacridone-type pigments occupies more than the 90% of the latter's annual production.Therefore as market is to quinoline
Acridine ketone pigment demand it is growing day by day, DMSS has shown the huge market space and wide
Development prospect.
The synthesis technique of DMSS is a lot, and mostly in the prior art is in higher boiling inert organic solvents
In, act on lower self-condensation with sodium methoxide or caustic alcohol with dimethyl succinate or diethyl succinate and be prepared from.In order to more
Good reaction effect, usually adds some polar latent solvents, and such as dimethylbenzene, dichloro-benzenes, DMF, dimethyl are sub-
Sulfone, sulfolane etc..Mentioned component, which participates in reaction, can cause the extension in reaction time, be asked while also there is product and be not easily purified etc.
Topic.In addition, the synthetic reaction of prior art is carried out in a batch manner, single batch of production is not only time-consuming longer, and high energy consumption, production capacity
It is low, it also there is the defects such as quality between batch is unstable.It is expected to overcome if it can develop a kind of synthetic method of successive reaction
Disadvantages described above.
The content of the invention
It is contemplated that for the technological deficiency of prior art, there is provided a kind of continuous production DMSS
Method, with solve in the prior art DMSS synthetic method batch-type carry out so that existence time length,
The technical problem of the low defect of high energy consumption, production capacity.
To realize above technical purpose, the present invention uses following technical scheme：
A kind of method of continuous production DMSS, comprises the following steps：
1) dimethyl succinate is taken, 100~110 DEG C, holding are heated under nitrogen guard mode and stirring condition
20min, then using dimethyl succinate and sodium methoxide amount ratio as 16:5(mL:G) succinic acid diformazan is added dropwise in ratio thereto
The methanol solution of ester and sodium methoxide, is continuously added dropwise under the conditions of 100~120 DEG C；
2) reactant is added drop-wise to after certain liquid level, it is continuous toward another reactor transfer material, obtain succinyl succinic acid
Diformazan ester sodium salt filter cake；
3) it is adjusted into pH to 2 with the dilution heat of sulfuric acid of 15-20% mass fractions, acidifying then filters reactant, and
Filter cake is washed afterwards, dried, that is, obtains DMSS.
Preferably, step 1) reacting environment be continuous reaction kettle.
Preferably, described be added dropwise, it is the ratio that dimethyl succinate and methanol solution of sodium methylate are controlled using flowmeter
Implement.
Preferably, step 3) in filtering obtained by filtrate be used for be distilled to recover dimethyl succinate.
The invention provides a kind of method of continuous production DMSS, the technical scheme is continuously to drip
Plus mode perform Claisen condensation reaction and the Michael Diekmann condensation reaction of dimethyl succinate and sodium methoxide, it is possible to achieve even
Continuous discharging, is acidified by dilute sulfuric acid, obtains DMSS again after collecting certain product.The present invention is based on classics
Experimental principle is designed, and the improvement of mode of operation forms brand-new technical process, and the technical scheme shortens the reaction time, simultaneously
Reduce energy consumption so that production efficiency is obviously improved, at the same overcome in batch production mode between different batches quality discrepancy compared with
Big the problem of.The present invention realizes good technique effect with innovative technological improvement, while cost is relatively low, be easily achieved,
Therefore with good promotion prospect.
Brief description of the drawings
Fig. 1 is the reaction principle figure of the inventive method.
Embodiment
The embodiment to the present invention is described in detail below.In order to avoid excessive unnecessary details,
It is will not be described in detail in following examples to belonging to known structure or function.
Approximating language used in following examples can be used for quantitative expression, show do not changing the feelings of basic function
Under condition quantity can be allowed to have certain variation.Therefore, it is accurate that the numerical value corrected with the language such as " about ", " left and right " is not limited to this
Numerical value is in itself.In certain embodiments, " about " represent the numerical value for allowing its amendment in the scope of positive and negative 10 (10%)
Interior change, such as, " about 100 " represent can be any numerical value between 90 to 110.In addition, " the about first numerical value is arrived
In the statement of second value ", the first and second numerical value two values are at about corrected.In some cases, approximating language
May be relevant with the precision of measuring instrument.
In addition to being defined, technology used and scientific terminology have and art technology people of the present invention in following examples
The identical meanings that member is commonly understood by.
Embodiment 1
A kind of method of continuous production DMSS, it is characterised in that comprise the following steps：
1) dimethyl succinate is taken, 105 DEG C, holding are heated under nitrogen guard mode and stirring condition
20min, then using dimethyl succinate and sodium methoxide amount ratio as 16:5(mL:G) succinic acid diformazan is added dropwise in ratio thereto
The methanol solution of ester and sodium methoxide, is continuously added dropwise under the conditions of 110 DEG C；
2) reactant is added drop-wise to after certain liquid level, continuous toward another reactor transfer material, insulation obtains succinyl fourth
Acid dimethyl sodium salt filter cake；
3) it is adjusted into pH to 2 with the dilution heat of sulfuric acid of 17% mass fraction, acidifying then filters reactant, then
Filter cake is washed, dried, that is, obtains DMSS.
On the basis of above technical scheme, following condition is met：
Step 1) reacting environment be continuous reaction kettle.
It is described to be added dropwise, it is to control the ratio of dimethyl succinate and methanol solution of sodium methylate to implement using flowmeter.
Step 3) in filtering obtained by filtrate be used for be distilled to recover dimethyl succinate.
Embodiment 2
A kind of method of continuous production DMSS, it is characterised in that comprise the following steps：
1) dimethyl succinate is taken, 100 DEG C, holding are heated under nitrogen guard mode and stirring condition
20min, then using dimethyl succinate and sodium methoxide amount ratio as 16:5(mL:G) succinic acid diformazan is added dropwise in ratio thereto
The methanol solution of ester and sodium methoxide, is continuously added dropwise under the conditions of 100 DEG C；
2) reactant is added drop-wise to after certain liquid level, continuous toward another reactor transfer material, insulation obtains succinyl fourth
Acid dimethyl sodium salt filter cake；
3) it is adjusted into pH to 2 with the dilution heat of sulfuric acid of 15% mass fraction, acidifying then filters reactant, then
Filter cake is washed, dried, that is, obtains DMSS.
Embodiment 3
A kind of method of continuous production DMSS, it is characterised in that comprise the following steps：
1) dimethyl succinate is taken, 110 DEG C, holding are heated under nitrogen guard mode and stirring condition
20min, then using dimethyl succinate and sodium methoxide amount ratio as 16:5(mL:G) succinic acid diformazan is added dropwise in ratio thereto
The methanol solution of ester and sodium methoxide, is continuously added dropwise under the conditions of 120 DEG C.
2) reactant is added drop-wise to after certain liquid level, continuous toward another reactor transfer material, insulation obtains succinyl fourth
Acid dimethyl sodium salt filter cake；
3) it is adjusted into pH to 2 with the dilution heat of sulfuric acid of 20% mass fraction, acidifying then filters reactant, then
Filter cake is washed, dried, that is, obtains DMSS.
Embodiments of the invention are described in detail above, but the content is only presently preferred embodiments of the present invention,
It is not intended to limit the invention.All any modifications, equivalent substitutions and improvements done in the application range of the present invention etc., all should
Within protection scope of the present invention.
Claims (4)
1. a kind of method of continuous production DMSS, it is characterised in that comprise the following steps：
1) dimethyl succinate is taken, 100~110 DEG C, holding are heated under nitrogen guard mode and stirring condition
20min, then using dimethyl succinate and sodium methoxide amount ratio as 16:5(mL:G) succinic acid diformazan is added dropwise in ratio thereto
The methanol solution of ester and sodium methoxide, is continuously added dropwise under the conditions of 100~120 DEG C；
2) reactant is added drop-wise to after certain liquid level, continuous toward another reactor transfer material, insulation obtains succinyl succinic acid
Diformazan ester sodium salt filter cake；
3) it is adjusted into pH to 2 with the dilution heat of sulfuric acid of 15-20% mass fractions, acidifying then filters reactant, then will
Filter cake washing, drying, that is, obtain DMSS.
2. a kind of method of continuous production DMSS according to claim 1, it is characterised in that step
Rapid reacting environment 1) is continuous reaction kettle.
3. a kind of method of continuous production DMSS according to claim 1, it is characterised in that institute
Dropwise addition is stated, is to control the ratio of dimethyl succinate and methanol solution of sodium methylate to implement using flowmeter.
4. a kind of method of continuous production DMSS according to claim 1, it is characterised in that step
Filtrate obtained by rapid 3) middle filtering is used to be distilled to recover dimethyl succinate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710409685.9A CN106986771A (en) | 2017-06-02 | 2017-06-02 | A kind of method of continuous production DMSS |
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| CN201710409685.9A CN106986771A (en) | 2017-06-02 | 2017-06-02 | A kind of method of continuous production DMSS |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108373412A (en) * | 2018-03-28 | 2018-08-07 | 彩客化学(沧州)有限公司 | The method and apparatus of continuous production dimethyl succinyl succinate |
| CN109824511A (en) * | 2019-04-09 | 2019-05-31 | 淄博鸿润新材料有限公司 | The preparation method of high-purity dimethyl succinyl succinate |
| CN112390717A (en) * | 2020-11-19 | 2021-02-23 | 江苏苏御新材料科技有限公司 | Preparation method of dimethyl succinylsuccinate |
| CN112592272A (en) * | 2020-12-23 | 2021-04-02 | 淄博鸿润新材料有限公司 | Environment-friendly production method for greatly reducing sewage discharge of dimethyl succinyl succinate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4435586A (en) * | 1982-04-28 | 1984-03-06 | Kruse Walter M | Etherification process for hexitols and anhydrohexitols |
| CN102093219A (en) * | 2010-11-22 | 2011-06-15 | 天津市职业大学 | Method for synthesizing succinyl succinic dialkyl ester |
-
2017
- 2017-06-02 CN CN201710409685.9A patent/CN106986771A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4435586A (en) * | 1982-04-28 | 1984-03-06 | Kruse Walter M | Etherification process for hexitols and anhydrohexitols |
| CN102093219A (en) * | 2010-11-22 | 2011-06-15 | 天津市职业大学 | Method for synthesizing succinyl succinic dialkyl ester |
Non-Patent Citations (2)
| Title |
|---|
| 郭玉良等: ""2，5-二氧-1，4-环己烷二甲酸二甲酯合成工艺研究"", 《精细化工》 * |
| 郭玉良等: ""丁二酰丁二酸二甲酯合成工艺研究"", 《天然气化工》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108373412A (en) * | 2018-03-28 | 2018-08-07 | 彩客化学(沧州)有限公司 | The method and apparatus of continuous production dimethyl succinyl succinate |
| CN108373412B (en) * | 2018-03-28 | 2021-08-03 | 彩客化学(沧州)有限公司 | Method and equipment for continuously producing dimethyl succinylsuccinate |
| CN109824511A (en) * | 2019-04-09 | 2019-05-31 | 淄博鸿润新材料有限公司 | The preparation method of high-purity dimethyl succinyl succinate |
| CN112390717A (en) * | 2020-11-19 | 2021-02-23 | 江苏苏御新材料科技有限公司 | Preparation method of dimethyl succinylsuccinate |
| CN112390717B (en) * | 2020-11-19 | 2022-08-09 | 江苏苏御新材料科技有限公司 | Preparation method of dimethyl succinylsuccinate |
| CN112592272A (en) * | 2020-12-23 | 2021-04-02 | 淄博鸿润新材料有限公司 | Environment-friendly production method for greatly reducing sewage discharge of dimethyl succinyl succinate |
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Application publication date: 20170728 |
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