CN110156565A - Trimethylolpropane extraction and water washing method - Google Patents

Trimethylolpropane extraction and water washing method Download PDF

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Publication number
CN110156565A
CN110156565A CN201910583562.6A CN201910583562A CN110156565A CN 110156565 A CN110156565 A CN 110156565A CN 201910583562 A CN201910583562 A CN 201910583562A CN 110156565 A CN110156565 A CN 110156565A
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China
Prior art keywords
phase
extraction
trimethylolpropane
washing
micro
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CN201910583562.6A
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Inventor
蒋国强
孙百亚
吴晓明
俞晔虎
姜伟伟
万鹏
梁国成
陶植
邹淼
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Jiangsu Baichuan Gaoke New Material Co ltd
Nantong Baichuan New Material Co ltd
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Jiangsu Baichuan Gaoke New Material Co ltd
Nantong Baichuan New Material Co ltd
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Priority to CN201910583562.6A priority Critical patent/CN110156565A/en
Publication of CN110156565A publication Critical patent/CN110156565A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/86Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention belongs to the technical field of fine chemical engineering, and particularly discloses a trimethylolpropane extraction and washing method, which comprises the following steps: and (3) extraction: extracting and separating trimethylolpropane by using a first micro-extractor to obtain an extract phase and a raffinate phase; washing with water: pumping the extracted phase and pure water into a second micro-extractor for primary washing and phase splitting to separate a first oil phase and a first water phase; the first water phase enters a first micro extractor, and the first oil phase enters a third micro extractor for secondary washing and phase separation, and is divided into a second water phase and a second oil phase again; the second water phase returns to the second micro-extractor for recycling, and the second oil phase obtains an organic phase containing sodium formate. The extraction and water washing method adopts a micro-channel extraction technology, and performs extraction and water washing on the trimethylolpropane for a plurality of times through the micro-extractor, so that the method has the advantages of convenient operation by personnel, low production energy consumption, convenient equipment heat preservation, low production cost and convenient realization, and the obtained product is superior to the traditional process.

Description

A kind of method of trimethylolpropane extraction washing
Technical field
The invention belongs to technical field of fine, the method for specifically a kind of trimethylolpropane extraction washing.
Background technique
Trimethylolpropane, alias are 2-2 dihydroxymethyl butanol, and molecular formula C6H14O3, No. CAS is 77-99-6, phase To molecular mass 134.17.Trimethylolpropane is mainly used for alkyd resin, polyurethane, unsaturated-resin, polyester resin, coating Equal fields are used for modifier and crosslinking agent for the manufacture of composite solidpropellant powder charge clad and heat insulation layer.Three hydroxyls Methylpropane night can be used for synthesizing aeroengine oil, printing ink etc., and trimethylolpropane also acts as textile auxiliary and polychlorostyrene The heat stabilizer of vinyl.
There are mainly two types of the synthetic methods of trimethylolpropane: condensation discrimination method and condensation hydrogenation method.Being condensed discrimination method is Traditional two-step synthesis method, this technics comparing is mature, but by-product is more, needs to consume a large amount of alkali, formaldehyde consumption is big, cost It is high.Condensation hydrogenation method is the two-step method to grow up the nineties, is first condensed repeated hydrogenation, can save the formaldehyde of one third and big The alkali of amount, by-product is relatively fewer, and purification is relatively simple, and equipment is few, at low cost, but this method to hydrogenation plant and is urged Agent is more demanding, is suitble to continuous production.
Condensation discrimination method is divided into calcium method and sodium method again.Wherein sodium method is i.e. using n-butanal and formaldehyde as raw material, with sodium hydroxide For catalyst, aldol reaction is carried out at a lower temperature and generates 2,2- dihydroxymethyl butyraldehyde, then with excessive formaldehyde and by force Alkali effect occurs Cannizzaro reaction and generates trimethylolpropane.Reaction equation are as follows:
Production process is (as shown in Figure 1): by the way that by n-butanal and formaldehyde, after condensation reaction generates liquid concentration, use is molten After agent extraction, washing, the trimethylolpropane extracting solution for being substantially free of sodium formate is obtained, extracting solution obtains after desolventizing Thick trimethylolpropane, thick trimethylolpropane are refined under a high vacuum again after first sloughing light component under a high vacuum, are obtained To qualified liquid trimethylolpropane.Sheet trimethylolpropane finished product is made by flaker in liquid trimethylolpropane.
At present in Conventional process, extraction washes extract using large-scale extraction tower, water scrubber and washes behaviour Make, the device is complicated, operating process condition is harsh, insulation of equipment is difficult, production process energy consumption is high, high production cost.
Summary of the invention
The object of the present invention is to provide a kind of methods of trimethylolpropane extraction washing, can be widely used in large-scale industry In production, mainly solving trimethylolpropane extraction washing in the prior art, the device is complicated, operating process condition is harsh, equipment is protected The problem of Wen Nan, production process energy consumption height, high production cost.
In order to solve the above technical problems, the present invention provides a kind of methods of trimethylolpropane extraction washing, including with Lower step:
The extraction of S1, trimethylolpropane:
Concentrate containing trimethylolpropane and extractant are proportionally added in the first micro-extraction apparatus;
Trimethylolpropane obtains extraction phase with raffinate phase after the first micro-extraction apparatus extraction and separation;
Raffinate phase enters sodium formate process units, and extraction phase enters washing step;
The washing of S2, trimethylolpropane:
Extraction phase and pure water are proportionally passed through into metering pump and squeeze into the second micro-extraction apparatus progress once washing, split-phase, point First oil phase and the first water phase out;
The first water phase that once washing, split-phase are got enters in the first micro-extraction apparatus, and the first oil mutually enters the micro- extraction of third Progress secondary washing, split-phase in device is taken, the second water phase and the second oily phase are again broken down into;
The second water phase that secondary washing, split-phase are got returns to recycling and reusing in the second micro-extraction apparatus, the second oily phase The organic phase for being substantially free of sodium formate is obtained, the sodium ions content in organic phase is measured.
Specifically, extractant is octanol in the S1.
Further, the ratio of the concentrate and extractant is 1:22~2.5.
Further, the ratio of extraction phase and pure water is 1:0.04~0.06 in the S2.
Specifically, the first oil mutually includes trimethylolpropane, extractant octanol and heavy component in the S2.
Specifically, the organic phase of the second oily phase includes trimethylolpropane, extractant octanol and heavy component in the S2.
The beneficial effects of the present invention are: the method for trimethylolpropane extraction washing of the present invention extracts skill using microchannel Art carries out extraction, washing several times to trimethylolpropane by simple equipment micro-extraction apparatus, reduces the organic phase of extraction In impurity content, improve the yield of trimethylolpropane, but also have personnel easy to operate, production energy consumption is low, and equipment is protected The characteristics of temperature is convenient, and production cost is low, is easy to implement, and obtained product is better than traditional handicraft.
Detailed description of the invention
It, below will be to required in embodiment or description of the prior art in order to illustrate more clearly of technical solution of the present invention The attached drawing used is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, right For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings Its attached drawing.
Fig. 1 is the flow sheet of trimethylolpropane in background technique;
Fig. 2 is the extraction of trimethylolpropane of the invention, washing process figure.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects It encloses.
In an embodiment of the present invention, a kind of method for specifically disclosing trimethylolpropane extraction washing, including it is following Step:
The extraction of S1, trimethylolpropane:
First micro- extraction is added according to the ratio of 1:22~2.5 in concentrate containing trimethylolpropane and extractant octanol It takes in device;
Trimethylolpropane obtains extraction phase with raffinate phase after the first micro-extraction apparatus extraction and separation;
Raffinate phase enters sodium formate process units, and extraction phase enters washing step;
The washing of S2, trimethylolpropane:
Extraction phase and pure water are squeezed into the second micro-extraction apparatus by metering pump according to the ratio of 1:0.04~0.06 and carry out one Secondary washing, split-phase separate the first oil phase and the first water phase;
The first water phase that once washing, split-phase are got enters in the first micro-extraction apparatus, and the first oil mutually enters the micro- extraction of third Progress secondary washing, split-phase in device is taken, is again broken down into the second water phase and the second oily phase, first oil mutually includes trihydroxy methyl third Alkane, extractant octanol and heavy component;
The second water phase that secondary washing, split-phase are got returns to recycling and reusing in the second micro-extraction apparatus, the second oily phase The organic phase for being substantially free of sodium formate is obtained, the sodium ions content in organic phase is measured, the organic phase of the described second oily phase includes Trimethylolpropane, extractant octanol and heavy component.
Embodiment 1:
The extraction process of S1, trimethylolpropane:
Concentrate and extractant octanol are squeezed into the first micro-extraction apparatus by metering pump according to 1:2.2 ratio;
Trimethylolpropane obtains extraction phase with raffinate phase after the first micro-extraction apparatus extraction and separation;Raffinate phase is contained The seldom aqueous sodium formate solution of machine object amount enters traditional sodium formate process units, measures content of organics therein and is 0.076%, raw material is provided to carry out the production of byproduct sodium formate, guarantees sodium formate product by measuring wherein content of organics Quality, because high organic content will affect the quality of sodium formate product;
Extraction phase carries out the processing of next step water-washing process, and raffinate phase carries out waste treatment;
S2, water-washing process:
Extraction phase and pure water be driven into the second micro-extraction apparatus according to 1:0.05 ratio by metering pump carry out once washing, Split-phase;
The first water phase that once washing, split-phase are got enters the first micro-extraction apparatus and carries out extracting operation again, once washing, The first oil that split-phase is got mutually enters third micro-extraction apparatus and carries out secondary washing, split-phase;
The second water phase that secondary washing, split-phase are got is used back to the recycling of the second micro-extraction apparatus;Secondary washing, split-phase point The second oil obtained mutually obtains the organic phase seldom containing sodium formate, and measuring sodium ions content therein is 54ppm.
Embodiment 2
The extraction process of S1, trimethylolpropane:
Concentrate and extractant octanol are squeezed into the first micro-extraction apparatus by metering pump according to 1:2.3 ratio;
Trimethylolpropane obtains extraction phase with raffinate phase after the first micro-extraction apparatus extraction and separation;Raffinate phase is contained The seldom aqueous sodium formate solution of machine object amount enters traditional sodium formate process units, measures content of organics therein and is 0.078%, raw material is provided to carry out the production of byproduct sodium formate, guarantees sodium formate product by measuring wherein content of organics Quality, because high organic content will affect the quality of sodium formate product;
Extraction phase carries out the processing of next step water-washing process, and raffinate phase carries out waste treatment;
S2, water-washing process:
Extraction phase and pure water be driven into the second micro-extraction apparatus according to 1:0.05 ratio by metering pump carry out once washing, Split-phase;
The first water phase that once washing, split-phase are got enters the first micro-extraction apparatus and carries out extracting operation again, once washing, The first oil that split-phase is got mutually enters third micro-extraction apparatus and carries out secondary washing, split-phase;
The second water phase that secondary washing, split-phase are got is used back to the recycling of the second micro-extraction apparatus;Secondary washing, split-phase point The second oil obtained mutually obtains the organic phase for being substantially free of sodium formate, and measuring sodium ions content therein is 36ppm.
Embodiment 3
The extraction process of S1, trimethylolpropane:
Concentrate and extractant octanol are squeezed into the first micro-extraction apparatus by metering pump according to 1:2.4 ratio;
Trimethylolpropane obtains extraction phase with raffinate phase after the first micro-extraction apparatus extraction and separation;Raffinate phase is contained The seldom aqueous sodium formate solution of machine object amount enters traditional sodium formate process units, measures content of organics therein and is 0.085%, raw material is provided to carry out the production of byproduct sodium formate, guarantees sodium formate product by measuring wherein content of organics Quality, because high organic content will affect the quality of sodium formate product;
Extraction phase carries out the processing of next step water-washing process, and raffinate phase carries out waste treatment;
S2, water-washing process:
Extraction phase and pure water be driven into the second micro-extraction apparatus according to 1:0.05 ratio by metering pump carry out once washing, Split-phase;
The first water phase that once washing, split-phase are got enters the first micro-extraction apparatus and carries out extracting operation again, once washing, The first oil that split-phase is got mutually enters third micro-extraction apparatus and carries out secondary washing, split-phase;
The second water phase that secondary washing, split-phase are got is used back to the recycling of the second micro-extraction apparatus;Secondary washing, split-phase point The second oil obtained mutually obtains the organic phase for being substantially free of sodium formate, and measuring sodium ions content therein is 18ppm.
Embodiment 4
The extraction process of S1, trimethylolpropane:
Concentrate and extractant octanol are squeezed into the first micro-extraction apparatus by metering pump according to 1:2.5 ratio;
Trimethylolpropane obtains extraction phase with raffinate phase after the first micro-extraction apparatus extraction and separation;Raffinate phase is contained The seldom aqueous sodium formate solution of machine object amount enters traditional sodium formate process units, measures content of organics therein and is 0.069%, raw material is provided to carry out the production of byproduct sodium formate, guarantees sodium formate product by measuring wherein content of organics Quality, because high organic content will affect the quality of sodium formate product;
Extraction phase carries out the processing of next step water-washing process, and raffinate phase carries out waste treatment;
S2, water-washing process:
Extraction phase and pure water be driven into the second micro-extraction apparatus according to 1:0.05 ratio by metering pump carry out once washing, Split-phase;
The first water phase that once washing, split-phase are got enters the first micro-extraction apparatus and carries out extracting operation again, once washing, The first oil that split-phase is got mutually enters third micro-extraction apparatus and carries out secondary washing, split-phase;
The second water phase that secondary washing, split-phase are got is used back to the recycling of the second micro-extraction apparatus;Secondary washing, split-phase point The second oil obtained mutually obtains the organic phase for being substantially free of sodium formate, and measuring sodium ions content therein is 14ppm.
Microchannel abstraction technique compared with traditional handicraft compared with:
Above disclosed be only a kind of preferred embodiment of the invention, cannot limit the present invention's certainly with this Interest field, therefore equivalent changes made in accordance with the claims of the present invention, are still within the scope of the present invention.

Claims (6)

1. a kind of method of trimethylolpropane extraction washing, which comprises the following steps:
The extraction of S1, trimethylolpropane:
Concentrate containing trimethylolpropane and extractant are proportionally added in the first micro-extraction apparatus;
Trimethylolpropane obtains extraction phase with raffinate phase after the first micro-extraction apparatus extraction and separation;
Raffinate phase enters sodium formate process units, and extraction phase enters washing step;
The washing of S2, trimethylolpropane:
It extraction phase and pure water is proportionally passed through into metering pump squeezes into the second micro-extraction apparatus and carry out once washing, split-phase, separate the One oil phase and the first water phase;
The first water phase that once washing, split-phase are got enters in the first micro-extraction apparatus, and the first oil mutually enters third micro-extraction apparatus Middle progress secondary washing, split-phase are again broken down into the second water phase and the second oily phase;
The second water phase that secondary washing, split-phase are got mutually is obtained back to recycling and reusing in the second micro-extraction apparatus, the second oil Organic phase measures the sodium ions content in organic phase.
2. a kind of method of trimethylolpropane extraction washing according to claim 1, which is characterized in that extract in the S1 Taking agent is octanol.
3. a kind of method of trimethylolpropane extraction washing according to claim 2, which is characterized in that the concentrate Ratio with extractant is 1:22~2.5.
4. a kind of method of trimethylolpropane extraction washing according to claim 1, which is characterized in that extract in the S2 Taking mutually is 1:0.04~0.06 with the ratio of pure water.
5. a kind of method of trimethylolpropane extraction washing according to claim 1, which is characterized in that the in the S2 One oil mutually includes trimethylolpropane, extractant octanol and heavy component.
6. a kind of method of trimethylolpropane extraction washing according to claim 1, which is characterized in that the in the S2 The organic phase of two oily phases includes trimethylolpropane, extractant octanol and heavy component.
CN201910583562.6A 2019-07-01 2019-07-01 Trimethylolpropane extraction and water washing method Pending CN110156565A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110563562A (en) * 2019-09-25 2019-12-13 南通百川新材料有限公司 extraction and water washing method of trimethylolpropane heavy component

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110563562A (en) * 2019-09-25 2019-12-13 南通百川新材料有限公司 extraction and water washing method of trimethylolpropane heavy component
CN110563562B (en) * 2019-09-25 2022-08-02 南通百川新材料有限公司 Extraction and water washing method of trimethylolpropane heavy component

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