CN108558601A - Pentaerythrite separation mother liquor prepares the device and preparation method thereof of liquid pentaerythrite - Google Patents
Pentaerythrite separation mother liquor prepares the device and preparation method thereof of liquid pentaerythrite Download PDFInfo
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- CN108558601A CN108558601A CN201810627273.7A CN201810627273A CN108558601A CN 108558601 A CN108558601 A CN 108558601A CN 201810627273 A CN201810627273 A CN 201810627273A CN 108558601 A CN108558601 A CN 108558601A
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- pentaerythrite
- mother liquor
- extractant
- extraction
- liquid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
Abstract
The present invention relates to the devices and preparation method thereof that a kind of pentaerythrite separation mother liquor prepares liquid pentaerythrite, it includes vaporising device that the pentaerythrite separation mother liquor, which prepares the device of liquid pentaerythrite, extraction equipment and rectifier unit, the pentaerythrite of the feed inlet connection pentaerythrite separation process of the vaporising device detaches mother liquor, discharge port connects extraction equipment, the extraction equipment is equipped with extractant adding mouth, for adding extractant into extraction equipment, after stratification to be mixed, extraction phase positioned at the extraction equipment top is pumped into rectifying in the rectifier unit and goes out extractant, the extractant that rectifying goes out enters extractant accumulator tank and is recycled.The present invention improves the quantum of output of separation process, while also reducing production cost, it is thus also avoided that the pollution of environment by the way that pentaerythrite separation mother liquor to be recycled into dehydration, extraction, rectification working process.
Description
Technical field
The present invention relates to pentaerythrite separation disposing mother liquor technical fields more particularly to a kind of pentaerythrite to detach mother liquor system
The device and preparation method thereof of standby liquid pentaerythrite.
Background technology
Currently, traditional pentaerythrite mother liquor is in point for isolating sodium formate or calcium formate, pentaerythrite, dipentaerythritol
After chaotropic, remaining separation mother liquor is generally handled by the way of burning, and detach in mother liquor also contain sodium formate or calcium formate,
Pentaerythrite, dipentaerythritol and liquid pentaerythrite (including pentaerythrite, dipentaerythritol, penta acetal of double seasons, three seasons penta
The mixture of acetal, lipid etc.), burning disposal not only pollutes environment, also causes waste.And liquid pentaerythrite is in alkyd tree
The reference of the fields such as fat, coating, ink, lubricating oil is extensive, the huge market demand.
Invention content
In view of the deficiencies of the prior art, the present invention provides the dress that a kind of pentaerythrite separation mother liquor prepares liquid pentaerythrite
Set and preparation method thereof, by the way that pentaerythrite separation mother liquor to be recycled into dehydration, extraction, rectification working process, improve
The quantum of output of separation process, while also reducing production cost, it is thus also avoided that the pollution of environment.
The technical solution adopted by the present invention to solve the technical problems is：The pentaerythrite separation mother liquor prepares liquid season
The device of penta tetrol includes vaporising device, extraction equipment and rectifier unit, and the feed inlet of the vaporising device connects pentaerythrite
The pentaerythrite of separation process detaches mother liquor, and discharge port connects extraction equipment, and the extraction equipment is equipped with extractant adding mouth,
For adding extractant into extraction equipment, after stratification to be mixed, the extraction phase for being located at the extraction equipment top is pumped into
Rectifying goes out extractant in the rectifier unit, and the extractant that rectifying goes out enters extractant accumulator tank and is recycled.
A kind of preferred embodiment of the device of liquid pentaerythrite is prepared in pentaerythrite provided by the invention separation mother liquor
In, the raffinate phase for being located at the extraction equipment lower part connects the separating liquid pipeline of pentaerythrite separation process by pipeline.
A kind of preferred embodiment of the device of liquid pentaerythrite is prepared in pentaerythrite provided by the invention separation mother liquor
In, the extractant uses one kind in organic solvent, including n-butanol, isobutanol, isooctanol, methanol, ethyl alcohol.
A kind of preferred embodiment of the device of liquid pentaerythrite is prepared in pentaerythrite provided by the invention separation mother liquor
In, the extraction equipment is using extraction kettle made of transparent material.
The preparation method that pentaerythrite separation mother liquor prepares liquid pentaerythrite includes the following steps：
Step 1：Dehydration, by pentaerythrite separation mother liquor be dehydrated using vaporising device, dehydration rate be 30%~
50%；
Step 2：Dewatered pentaerythrite separation mother liquor in extraction equipment is added extractant, is stirred by extraction
Stratification is handled afterwards, obtains the raffinate phase positioned at the extraction phase on extraction equipment top and positioned at extraction equipment lower part；
Step 3：Extraction phase is pumped into rectifier unit and carries out rectifying by rectifying, and the extractant that rectifying goes out enters extractant and returns
It receives slot to recycle, rectifying raffinate, that is, liquid pentaerythrite.
A kind of preferable reality of the preparation method of liquid pentaerythrite is prepared in pentaerythrite provided by the invention separation mother liquor
It applies in example, the additive amount of the extractant is 1~10 times that pentaerythrite detaches mother liquor.
Compared with prior art, pentaerythrite provided by the invention separation mother liquor prepare liquid pentaerythrite device and its
The advantageous effect of preparation method is：The present invention is by pentaerythrite separation mother liquor successively into dehydration, extraction processing, the extraction phase of extraction
Go out extractant through rectification working process rectifying, remaining as liquid pentaerythrite, the liquid pentaerythrite of pentaerythrite separation mother liquor is made to receive
Rate reaches 10%, and raffinate phase then enters the separating liquid pipeline of pentaerythrite separation process, increases the quantum of output of separating liquid, makes production
500-800 yuan/ton of cost reduction, can generate the economic benefit of ten thousand yuan of 200-350 every year.
Description of the drawings
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing, wherein：
Fig. 1 is the structure principle chart for the device that pentaerythrite separation mother liquor provided by the invention prepares liquid pentaerythrite.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that the described embodiments are merely a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts all other
Embodiment shall fall within the protection scope of the present invention.
Referring to Fig. 1, the device 1 that pentaerythrite separation mother liquor prepares liquid pentaerythrite include vaporising device 11,
Extraction equipment 12 and rectifier unit 13, the pentaerythrite of the feed inlet connection pentaerythrite separation process 14 of the vaporising device 11
Mother liquor 141 is detached, discharge port connects extraction equipment 12, and the extraction equipment 12 is equipped with extractant adding mouth 122, is used for extraction
It takes and adds extractant in device 12, after stratification to be mixed, be located at described in the extraction phase suction on 12 top of the extraction equipment
Rectifying goes out extractant in rectifier unit 13, and the extractant that rectifying goes out enters extractant accumulator tank 15 and is recycled.
Further, the raffinate phase for being located at 12 lower part of the extraction equipment connects pentaerythrite separation process 14 by pipeline
Separating liquid pipeline 142.
Specifically, the extractant is using in organic solvent, including n-butanol, isobutanol, isooctanol, methanol, ethyl alcohol
It is a kind of.
Preferably, the extraction equipment 12 is using extraction kettle made of transparent material.
Embodiment one：
Step 1：Dehydration takes pentaerythrite to detach mother liquor 100mL, and it is 30% to carry out dehydration rate by vaporising device 11
Dehydration；
Step 2：The extraction of 200mL is added in dewatered pentaerythrite separation mother liquor by extraction in extraction equipment 12
Agent is stirred 3h, stands 2h, obtains the raffinate positioned at the extraction phase on 12 top of extraction equipment and positioned at extraction equipment lower part
Phase, wherein extraction phase are mainly extractant, pentaerythrite, dipentaerythritol, penta acetal of double seasons, three seasons, penta acetal, lipid etc.
Mixture, raffinate phase are mainly sodium formate or calcium formate, pentaerythrite, dipentaerythritol；
Step 3：Rectifying is extracted in extraction phase to rectifier unit 13, and rectifying goes out extractant, obtains the liquid season of about 20mL
Penta tetrol, the separating liquid pipeline 142 that raffinate phase then enters pentaerythrite separation process 14 recycle.
Embodiment two：
Step 1：Dehydration takes pentaerythrite to detach mother liquor 100mL, and it is 40% to carry out dehydration rate by vaporising device 11
Dehydration；
Step 2：The extraction of 300mL is added in dewatered pentaerythrite separation mother liquor by extraction in extraction equipment 12
Agent is stirred 3h, stands 2h, obtains the raffinate positioned at the extraction phase on 12 top of extraction equipment and positioned at extraction equipment lower part
Phase, wherein extraction phase are mainly extractant, pentaerythrite, dipentaerythritol, penta acetal of double seasons, three seasons, penta acetal, lipid etc.
Mixture, raffinate phase are mainly sodium formate or calcium formate, pentaerythrite, dipentaerythritol；
Step 3：Rectifying is extracted in extraction phase to rectifier unit 13, and rectifying goes out extractant, obtains the liquid season of about 30mL
Penta tetrol, the separating liquid pipeline 142 that raffinate phase then enters pentaerythrite separation process 14 recycle.
Embodiment three：
Step 1：Dehydration takes pentaerythrite to detach mother liquor 100mL, and it is 50% to carry out dehydration rate by vaporising device 11
Dehydration；
Step 2：The extraction of 500mL is added in dewatered pentaerythrite separation mother liquor by extraction in extraction equipment 12
Agent is stirred 3h, stands 2h, obtains the raffinate positioned at the extraction phase on 12 top of extraction equipment and positioned at extraction equipment lower part
Phase, wherein extraction phase are mainly extractant, pentaerythrite, dipentaerythritol, penta acetal of double seasons, three seasons, penta acetal, lipid etc.
Mixture, raffinate phase are mainly sodium formate or calcium formate, pentaerythrite, dipentaerythritol；
Step 3：Rectifying is extracted in extraction phase to rectifier unit 13, and rectifying goes out extractant, obtains the liquid season of about 35mL
Penta tetrol, the separating liquid pipeline 142 that raffinate phase then enters pentaerythrite separation process 14 recycle.
Pentaerythrite separation mother liquor provided by the invention prepares the beneficial of device of liquid pentaerythrite and preparation method thereof
Effect is：The present invention is by pentaerythrite separation mother liquor successively into dehydration, extraction processing, and the extraction phase of extraction is through rectification working process rectifying
Go out extractant, remaining as liquid pentaerythrite, so that the liquid pentaerythrite yield of pentaerythrite separation mother liquor is reached 10%, raffinate
Phase then enters the separating liquid pipeline of pentaerythrite separation process, increases the quantum of output of separating liquid, production cost is made to reduce 500-
800 yuan/ton, the economic benefit of ten thousand yuan of 200-350 can be generated every year.
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to utilize this hair
Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks
Domain is similarly included within the scope of patent protection of the present invention.
Claims (6)
1. a kind of pentaerythrite separation mother liquor prepares the device of liquid pentaerythrite, it is characterised in that：Including vaporising device, extraction
The pentaerythrite of device and rectifier unit, the feed inlet connection pentaerythrite separation process of the vaporising device detaches mother liquor, goes out
Material mouth connects extraction equipment, and the extraction equipment is waited for equipped with extractant adding mouth for adding extractant into extraction equipment
After stirring stratification, the extraction phase positioned at the extraction equipment top is pumped into rectifying in the rectifier unit and goes out extractant, essence
The extractant distillated enters extractant accumulator tank and is recycled.
2. pentaerythrite separation mother liquor according to claim 1 prepares the device of liquid pentaerythrite, it is characterised in that：Position
The separating liquid pipeline that raffinate phase in the extraction equipment lower part passes through pipeline connection pentaerythrite separation process.
3. pentaerythrite separation mother liquor according to claim 1 prepares the device of liquid pentaerythrite, it is characterised in that：Institute
Extractant is stated using one kind in organic solvent, including n-butanol, isobutanol, isooctanol, methanol, ethyl alcohol.
4. pentaerythrite separation mother liquor according to claim 1 prepares the device of liquid pentaerythrite, it is characterised in that：Institute
Extraction equipment is stated using extraction kettle made of transparent material.
5. pentaerythrite separation mother liquor according to any one of claims 1 to 4 prepares the preparation method of liquid pentaerythrite,
It is characterized in that：Include the following steps：
Step 1：Pentaerythrite separation mother liquor is dehydrated by dehydration using vaporising device, and dehydration rate is 30%~50%；
Step 2：Dewatered pentaerythrite separation mother liquor in extraction equipment is added extractant, is stirred rear quiet by extraction
Layered shaping is set, the raffinate phase positioned at the extraction phase on extraction equipment top and positioned at extraction equipment lower part is obtained；
Step 3：Extraction phase is pumped into rectifier unit and carries out rectifying by rectifying, and the extractant that rectifying goes out enters extractant accumulator tank
It recycles, rectifying raffinate, that is, liquid pentaerythrite.
6. pentaerythrite separation mother liquor according to claim 5 prepares the preparation method of liquid pentaerythrite, feature exists
In：The additive amount of the extractant is 1~10 times that pentaerythrite detaches mother liquor.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810627273.7A CN108558601A (en) | 2018-06-19 | 2018-06-19 | Pentaerythrite separation mother liquor prepares the device and preparation method thereof of liquid pentaerythrite |
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| CN201810627273.7A CN108558601A (en) | 2018-06-19 | 2018-06-19 | Pentaerythrite separation mother liquor prepares the device and preparation method thereof of liquid pentaerythrite |
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| CN108558601A true CN108558601A (en) | 2018-09-21 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113336625A (en) * | 2021-06-07 | 2021-09-03 | 内蒙古宜化化工有限公司 | Method for treating pentaerythritol mother liquor |
Citations (4)
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|---|---|---|---|---|
| CN1254702A (en) * | 1998-11-21 | 2000-05-31 | 衡阳三化实业股份有限公司 | Process for recovering pentaerythritol and protan from mother liquid of pentaerythritol |
| CN101012156A (en) * | 2007-02-13 | 2007-08-08 | 濮阳市永安化工有限公司 | Process of preparing dipentaerythritol and/or tripentaerythritol |
| CN102617323A (en) * | 2012-03-05 | 2012-08-01 | 贵州金江化工有限公司 | Method for recovering pentaerythritol and sodium formate |
| CN106748738A (en) * | 2015-11-25 | 2017-05-31 | 衡阳屹顺化工有限公司 | A kind of Optimized Extraction technique of separating formic sodium |
-
2018
- 2018-06-19 CN CN201810627273.7A patent/CN108558601A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1254702A (en) * | 1998-11-21 | 2000-05-31 | 衡阳三化实业股份有限公司 | Process for recovering pentaerythritol and protan from mother liquid of pentaerythritol |
| CN101012156A (en) * | 2007-02-13 | 2007-08-08 | 濮阳市永安化工有限公司 | Process of preparing dipentaerythritol and/or tripentaerythritol |
| CN102617323A (en) * | 2012-03-05 | 2012-08-01 | 贵州金江化工有限公司 | Method for recovering pentaerythritol and sodium formate |
| CN106748738A (en) * | 2015-11-25 | 2017-05-31 | 衡阳屹顺化工有限公司 | A kind of Optimized Extraction technique of separating formic sodium |
Non-Patent Citations (2)
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| 宣晓君: "季戊四醇母液回收" * |
| 李忠玉: "从季戊四醇母液中分离季戊四醇与甲酸钠的研究" * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113336625A (en) * | 2021-06-07 | 2021-09-03 | 内蒙古宜化化工有限公司 | Method for treating pentaerythritol mother liquor |
| CN113336625B (en) * | 2021-06-07 | 2023-11-07 | 内蒙古宜化化工有限公司 | Treatment method of pentaerythritol mother liquor |
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