CN103360213B - Chloropropanediol purifying apparatus and production method thereof - Google Patents

Chloropropanediol purifying apparatus and production method thereof Download PDF

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Publication number
CN103360213B
CN103360213B CN201310323361.5A CN201310323361A CN103360213B CN 103360213 B CN103360213 B CN 103360213B CN 201310323361 A CN201310323361 A CN 201310323361A CN 103360213 B CN103360213 B CN 103360213B
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tank
reaction
header tank
hydrolysis kettle
ion exchange
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CN103360213A (en
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郭学阳
张志刚
王欣鹏
刘见齐
楚希玲
李绍彦
李绍禹
左言恺
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WEIFANG WORLD TECHNOLOGY CO., LTD.
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WEIFANG WORLD CHEMICAL CO Ltd
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Abstract

The invention discloses a chloropropanediol purifying apparatus and a production method thereof. The apparatus comprises a hydrolysis kettle, a hydrolysate header tank, ion exchange columns, a distillation still and a condenser which are connected through a pipeline, the output pipeline of the condenser is connected with a front fraction pot and a finished product pot, and the front fraction pot and the finished product pot are respectively connected with a vacuum set. The production method comprises the following steps: respectively pumping softened water, sulfuric acid and an aqueous solution of p-toluenesulfonic acid into the hydrolysis kettle according to a ratio, stirring, heating, adding chloropropylene oxide to the hydrolysis kettle for a reaction, and continuously heating for a new reaction after reaction ending; putting the obtained hydrolysate in the ion exchange columns for ion exchange; adding the obtained ion exchange liquid to the distillation kettle, starting stirring, carrying out steam heating, and starting a hydraulic jet vacuum pump; stopping the hydraulic jet vacuum pump when there is no liquid drop between the condenser and a reception pot, and sequentially starting roots vacuum sets; and conveying the obtained material to the front fraction pot, and switching the front fraction pot to the finished product pot.

Description

A kind of glycerin chlorohydrin purifying plant and production method thereof
Technical field
The present invention relates to a kind of production method of glycerin chlorohydrin, specifically, relate to a kind of glycerin chlorohydrin purifying plant and production method thereof, belong to chemical technology field.
Background technology
Contain-Cl group and two hydroxyls in glycerin chlorohydrin (chemical name 3-chlorine-1,2-propylene glycol) molecule, its structural performance has determined that it is a kind of valuable chemical intermediate.As medicine intermediate, for the production of eliminating phlegm, go to cough medicine guaiacol glycerol ether, suppressing panting calming medicine theophylline, proxyphylline, produces non-ionic contrast agent Schering AG), ioversol etc.; As basic material, produce softening agent, tensio-active agent, dyestuff etc.; Synthetic self-extinguishing epoxy resin together with two-(p-hydroxyphenyl)-trichloroethane; Also as solvent, for the production of cellulose acetate etc.In recent years, the research that the synthetic medicine of glycerin chlorohydrin especially affects in life science aspect the male sex's reproductive function was very active, constantly had new results to come out.
At present, the synthetic method of glycerin chlorohydrin mainly contains: epoxy chloropropane hydrolysis, glycerin chlorination method, vinyl carbinol oxychlorination method etc.Glycerin chlorination explained hereafter glycerin chlorohydrin cost is lower, but investment is larger, and by-product dilute hydrochloric acid, and in glycerin chlorohydrin product, foreign matter content is high, has many chlorinated compounds and polymolecular polymkeric substance etc., has affected use synthetic at medicine, civil goods field; Glycerin chlorohydrin product purity prepared by epoxy chloropropane hydrolysis process is higher, but in industry, has the problems such as yield is low, of poor benefits at present; The investment of vinyl carbinol oxychlorination method is huge, and the product of preparation also exists the problems such as purity is low.Consider the factors such as Technological Economy, optimizing epoxy chloropropane hydrolysis process production high purity glycerin chlorohydrin has important economic implications and social effect.
Summary of the invention
The problem to be solved in the present invention is that in the production existing for domestic glycerin chlorohydrin industry, product purity is low, foreign matter content is high, feed stock conversion is low, product yield is low, deficiency in economic performance, improved yield and the cost problem that raises etc., provide a kind of and can improve product purity, the glycerin chlorohydrin purifying plant of the waste residue amount producing in reduction amount of impurities and content, minimizing production, the product cost that reduces, raising product economy benefit, shortening production cycle, raising plant factor.
In order to address the above problem, the present invention by the following technical solutions:
A kind of glycerin chlorohydrin purifying plant, comprise successively by hydrolysis kettle, hydrolyzed solution header tank, ion exchange column, still kettle, the condenser of pipeline connection, on the delivery conduit of described condenser, be connected with front-end volatiles tank and finished pot, front-end volatiles tank and finished pot are connected with respectively vacuum unit.
Below the further optimization of the present invention to above-mentioned division:
Between the lower end of described hydrolysis kettle and upper end, circulation line is installed, recycle pump is installed on circulation line.
On circulation line, be connected with glass condenser; The liquid-inlet pipe of hydrolyzed solution header tank is communicated with circulation line.
The top of hydrolysis kettle is communicated with header tank.
The production method that the present invention also provides a kind of glycerin chlorohydrin to purify, this production method comprises the following steps:
A, by softening water, sulfuric acid, the tosic acid aqueous solution respectively according to proportioning suction hydrolysis kettle, after stirring, open steam and heat up, by epoxy chloropropane suction header tank, from header tank to hydrolysis kettle, add epoxy chloropropane to react, after completion of the reaction, continue temperature reaction;
B, with recycle pump, hydrolyzed solution is squeezed into hydrolyzed solution header tank after completion of the reaction, then put into ion exchange column and carry out ion-exchange;
C, the ion exchange liquid being comprised of water, glycerin chlorohydrin is added to still kettle, open and stir, open steam and heat up, then open waterpower ejector vacuum pump;
D, when observing condenser and occur depending on cup dripless to receiving tank, close hydrojet vacuum pump, open successively Roots vacuum system; Mass transport, to front-end volatiles tank, and is switched to finished pot by front-end volatiles tank.
The further optimization of the present invention to such scheme below:
In described steps A: chemical equation is:
Main reaction
Side reaction
Epoxy chlorine alkane hydrin.
Further optimize: in described steps A, first by vacuum by epoxy chloropropane suction header tank, by softening water, sulfuric acid, according to proportioning tosic acid (being made into 10% aqueous solution) suction hydrolysis kettle, ON cycle pump, stir after 30-40 minute, open steam and heat up, in 30-40 minute, be raised to 70-75 ℃; From header tank, to hydrolysis kettle, add epoxy chloropropane, within 2-3 hour, add, during to control temperature of reaction be 86-93 ℃, react complete, be warming up to 94-102 ℃ and continue reaction 2-3 hour.
Further optimize: in described step B, first hydrolysis kettle is cooled to 30-40 ℃, then with recycle pump, hydrolyzed solution is squeezed into hydrolyzed solution header tank, then put into ion exchange column, adjusting rate of discharge is 0.3-0.4m 3/ h.
Further optimize: in described step C, first ion exchange liquid is added to still kettle, open and stir, open steam and heat up; First boil off moisture, before 101 ℃ of gas phase temperatures, phlegma returns hydrolysis kettle as moisture and continues to use;
When gas phase temperature surpasses 101 ℃, open waterpower ejector vacuum pump, control vacuum tightness is 0.094-0.096MPa.
Further optimize: in described step D, when observing condenser and occur depending on cup dripless to receiving tank, close hydrojet vacuum pump, open successively Roots vacuum system; Gas phase temperature is front-end volatiles lower than the phlegma of 90 ℃, when gas phase temperature surpasses 0.099MPa since 90 ℃ of in rising trend, system vacuum degree, material is switched to finished pot by front-end volatiles tank.
The present invention adopts such scheme, has the following advantages:
1, main raw material epoxy chloropropane is shape spray and adds hydrolysis kettle, increase with softening water contact area, and sufficient reacting, reaction effect is good; Side reaction reduces, and by product reduces;
2, adopt recycle pump that the material in reaction process is beaten to circulation, hydrolysis kettle internal upper part, middle part, bottom hydrolysis reaction process are almost consistent, and material reaction homogeneity strengthens;
3, with pump, material is added from glass condenser return line, gas material is upwards operation from glass condenser return line lower end, liquid material contacts with gas material is reverse, after moment mass-and heat-transfer, return hydrolysis kettle and continue reaction, reduce volatilization and the loss of material, improved the utilization ratio of raw material;
4, adopt sulfuric acid, tosic acid dual-component catalyst, hydrolysis sulfuric acid catalysis activity in early stage is stronger, and hydrolysis later stage Catalyzed by p-Toluenesulfonic Acid activity is stronger, and two kinds of catalyst effects complement each other, and hydrolysis reaction speed is accelerated, and epoxy chloropropane transformation efficiency improves.
5, adopt ion exchange resin to remove the impurity in hydrolyzed solution, saved and in existing technique, used in alkali and wait operation, ion exchange liquid obtains the glycerin chlorohydrin that purity is very high, product application range extension after distilling according to set rules.
6, adopt the water ring-Roots vacuum system of high vacuum to distill, gaseous state glycerin chlorohydrin velocity of evaporation is fast, liquid phase and gas phase temperature are low, the amount of liquid phase material thermo-cracking, polymerization and generation pungency propenal greatly reduces, finished product glycerin chlorohydrin yield is brought up to 110%(method of calculation: the glycerin chlorohydrin amount of generation is divided by the epoxy chloropropane amount dropping into), glycerin chlorohydrin content surpasses 99.6%.
Accompanying drawing explanation
Accompanying drawing 1 is the structural representation of glycerin chlorohydrin purifying plant in the embodiment of the present invention.
In figure: 1-header tank; 2-glass condenser; 3-hydrolysis kettle; 4-recycle pump; 5-hydrolyzed solution header tank; 6-ion exchange column; 7-still kettle; 8-condenser; 9-finished pot; 10-front-end volatiles tank.
Embodiment
Embodiment 1, as shown in Figure 1, a kind of glycerin chlorohydrin purifying plant, comprise successively by hydrolysis kettle 3, hydrolyzed solution header tank 5, ion exchange column 6, still kettle 7, the condenser 8 of pipeline connection, on the delivery conduit of described condenser 8, be connected with front-end volatiles tank 10 and finished pot 9, front-end volatiles tank 10 and finished pot 9 are connected with respectively vacuum unit.
Between the lower end of described hydrolysis kettle 3 and upper end, circulation line is installed, recycle pump 4 is installed on circulation line.
On circulation line, be connected with glass condenser 2; The liquid-inlet pipe of hydrolyzed solution header tank 5 is communicated with circulation line.
The top of hydrolysis kettle 3 is communicated with header tank 1, on header tank 1, by pipeline, is connected with hydrojet vacuum pump.
Connecting pipeline between header tank 1 and hydrojet vacuum pump is communicated with the connecting pipeline between front-end volatiles tank 10, finished pot 9 and vacuum unit.
The production method that this glycerin chlorohydrin is purified comprises the following steps:
A, by vacuum by 300Kg epoxy chloropropane suction header tank 1, by 600Kg softening water, 2.2Kg sulfuric acid, 1.5Kg tosic acid (being made into 10% aqueous solution) suction hydrolysis kettle 3, ON cycle pump 4, stirs after 30 minutes, open steam and heat up, in 40 minutes, be raised to 70 ℃.From header tank 1, to hydrolysis kettle 3, add epoxy chloropropane, within 2.5 hours, add, during to control temperature of reaction be 89-93 ℃.React complete, be warming up to 95-99 ℃ and continue reaction 2 hours.
Main reaction
Side reaction
Epoxy chlorine alkane hydrin;
B, hydrolysis kettle 3 is cooled to 35 ℃, with recycle pump 4, hydrolyzed solution is squeezed into hydrolyzed solution header tank 5, then put into ion exchange column 6, adjusting rate of discharge is 0.35m 3/ h.
Zeo-karb is housed in ion exchange column, on this resin structure, has Na +.In the hydrolyzed solution that reaction generates, contain impurity as acidic substance (example hydrochloric acid, molecular structure HCl) and other positively ionized compound containing macromolecular structure.Hydrolyzed solution enters after ion exchange column, the positively ionized compound in hydrolyzed solution and the Na on resin structure +exchange, the impurity such as pigment in hydrolyzed solution are removed in absorption simultaneously.After exchange, in hydrolyzed solution, foreign matter content reduces, and from ion-exchange column bottom, exchange liquid main component is out water, glycerin chlorohydrin.
C, ion exchange liquid is added to still kettle 7, open and stir, open steam and heat up.First boil off moisture, before 101 ℃ of gas phase temperatures, phlegma returns hydrolysis kettle 3 as moisture and continues to use.
When gas phase temperature surpasses 101 ℃, open waterpower ejector vacuum pump, control vacuum tightness is 0.094MPa.
D, when observing condenser 8 and occur depending on cup dripless to receiving tank, close hydrojet vacuum pump, open successively Roots vacuum system.
Gas phase temperature is front-end volatiles lower than the phlegma of 90 ℃.When gas phase temperature surpasses 0.099Mpa since 90 ℃ of in rising trend, system vacuum degree, material is switched to finished pot 9 by front-end volatiles tank 10.
It in finished pot 9, is finished product glycerin chlorohydrin; Composition in front-end volatiles tank 10 is: a small amount of glycerin chlorohydrin, moisture and the dichloro-glycerine of carrying secretly out on a small quantity, a small amount of boiling point is lower than the compound of glycerin chlorohydrin etc.
The product quality indicator of preparation is in Table 1
Table 1 product quality analysis result
Embodiment 2, as shown in Figure 1, a kind of glycerin chlorohydrin purifying plant, comprise successively by hydrolysis kettle 3, hydrolyzed solution header tank 5, ion exchange column 6, still kettle 7, the condenser 8 of pipeline connection, on the delivery conduit of described condenser 8, be connected with front-end volatiles tank 10 and finished pot 9, front-end volatiles tank 10 and finished pot 9 are connected with respectively vacuum unit.
Between the lower end of described hydrolysis kettle 3 and upper end, circulation line is installed, recycle pump 4 is installed on circulation line.
On circulation line, be connected with glass condenser 2; The liquid-inlet pipe of hydrolyzed solution header tank 5 is communicated with circulation line.
The top of hydrolysis kettle 3 is communicated with header tank 1, on header tank 1, by pipeline, is connected with hydrojet vacuum pump.
Connecting pipeline between header tank 1 and hydrojet vacuum pump is communicated with the connecting pipeline between front-end volatiles tank 10, finished pot 9 and vacuum unit.
The production method that this glycerin chlorohydrin is purified comprises the following steps:
A, by vacuum by 250Kg epoxy chloropropane suction header tank, by 620Kg softening water, 2.4Kg sulfuric acid, 1.6Kg tosic acid (being made into 10% aqueous solution) suction hydrolysis kettle, ON cycle pump, stirred after 40 minutes, opened steam and heated up, and in 30 minutes, was raised to 72 ℃.From header tank, to hydrolysis kettle, add epoxy chloropropane, within 3 hours, add, during to control temperature of reaction be 86-92 ℃.React complete, be warming up to 94-98 ℃ and continue reaction 3 hours.
Main reaction
Side reaction
Epoxy chlorine alkane hydrin;
B, hydrolysis kettle is cooled to 40 ℃, with pump, squeezes into hydrolyzed solution header tank, then put into ion exchange column, adjusting rate of discharge is 0.3m 3/ h.
C, ion exchange liquid is added to still kettle, open and stir, open steam and heat up.First boil off moisture, before 101 ℃ of gas phase temperatures, phlegma returns hydrolysis kettle as moisture and continues to use.When gas phase temperature surpasses 101 ℃, open waterpower ejector vacuum pump, control vacuum tightness is 0.095MPa.
D, when observing condenser and occur depending on cup dripless to receiving tank, close hydrojet vacuum pump, open successively Roots vacuum system.Gas phase temperature is front-end volatiles lower than the phlegma of 90 ℃.When gas phase temperature surpasses 0.099MPa since 90 ℃ of in rising trend, system vacuum degree, material is switched to finished pot by front-end volatiles tank.
The product quality indicator of preparation is in Table 2.
Table 2 product quality analysis result
Interventions Requested Analytical results
Outward appearance Water white transparency thick liquid
Glycerin chlorohydrin content, (GC) % 99.61
Foreign matter content, (GC) % before glycerin chlorohydrin main peak 0.13
Glycerin chlorohydrin main peak rear impurity content, (GC) % 0.26
Embodiment 3, as shown in Figure 1, a kind of glycerin chlorohydrin purifying plant, comprise successively by hydrolysis kettle 3, hydrolyzed solution header tank 5, ion exchange column 6, still kettle 7, the condenser 8 of pipeline connection, on the delivery conduit of described condenser 8, be connected with front-end volatiles tank 10 and finished pot 9, front-end volatiles tank 10 and finished pot 9 are connected with respectively vacuum unit.
Between the lower end of described hydrolysis kettle 3 and upper end, circulation line is installed, recycle pump 4 is installed on circulation line.
On circulation line, be connected with glass condenser 2; The liquid-inlet pipe of hydrolyzed solution header tank 5 is communicated with circulation line.
The top of hydrolysis kettle 3 is communicated with header tank 1, on header tank 1, by pipeline, is connected with hydrojet vacuum pump.
Connecting pipeline between header tank 1 and hydrojet vacuum pump is communicated with the connecting pipeline between front-end volatiles tank 10, finished pot 9 and vacuum unit.
The production method that this glycerin chlorohydrin is purified comprises the following steps:
A, by vacuum by 280Kg epoxy chloropropane suction header tank, by 660Kg softening water, 2.6Kg sulfuric acid, 3.2Kg tosic acid (being made into 10% aqueous solution) suction hydrolysis kettle, ON cycle pump, stirs after 35 minutes, open steam and heat up, in 40 minutes, be raised to 75 ℃.From header tank, to hydrolysis kettle, add epoxy chloropropane, within 2.5 hours, add, during to control temperature of reaction be 86-92 ℃.React complete, be warming up to 98-102 ℃ and continue reaction 3 hours.
Main reaction
Side reaction
Epoxy chlorine alkane hydrin;
B, hydrolysis kettle is cooled to 30 ℃, with pump, squeezes into hydrolyzed solution header tank, then put into ion exchange column, adjusting rate of discharge is 0.4m 3/ h.
C, ion exchange liquid is added to still kettle, open and stir, open steam and heat up.First boil off moisture, before 101 ℃ of gas phase temperatures, phlegma returns hydrolysis kettle as moisture and continues to use.When gas phase temperature surpasses 101 ℃, open waterpower ejector vacuum pump, control vacuum tightness is 0.096MPa.
D, when observing condenser and occur depending on cup dripless to receiving tank, close hydrojet vacuum pump, open successively Roots vacuum system.Gas phase temperature is front-end volatiles lower than the phlegma of 90 ℃.When gas phase temperature surpasses 0.099MPa since 90 ℃ of in rising trend, system vacuum degree, material is switched to finished pot by front-end volatiles tank.
The product quality indicator of preparation is in Table 3.
Table 3 product quality analysis result
Interventions Requested Analytical results
Outward appearance Water white transparency thick liquid
Glycerin chlorohydrin content, (GC) % 99.62
Foreign matter content, (GC) % before glycerin chlorohydrin main peak 0.10
Glycerin chlorohydrin main peak rear impurity content, (GC) % 0.28

Claims (2)

1. a glycerin chlorohydrin purifying plant, it is characterized in that: this device comprises successively by hydrolysis kettle (3), hydrolyzed solution header tank (5), ion exchange column (6), still kettle (7), the condenser (8) of pipeline connection, on the delivery conduit of described condenser (8), be connected with front-end volatiles tank (10) and finished pot (9), front-end volatiles tank (10) and finished pot (9) are connected with respectively vacuum unit;
Between the lower end of described hydrolysis kettle (3) and upper end, circulation line is installed, recycle pump (4) is installed on circulation line; On circulation line, be connected with glass condenser (2); The liquid-inlet pipe of hydrolyzed solution header tank (5) is communicated with circulation line;
The top of hydrolysis kettle (3) is communicated with header tank (1).
2. the production method that glycerin chlorohydrin is purified, is characterized in that: the method comprises the following steps:
A, by softening water, sulfuric acid, the tosic acid aqueous solution respectively according to proportioning suction hydrolysis kettle (3), after stirring, opening steam heats up, by epoxy chloropropane suction header tank (1), from header tank (1), to hydrolysis kettle (3), add epoxy chloropropane to react, after completion of the reaction, continue temperature reaction;
First by vacuum by epoxy chloropropane suction header tank (1), by softening water, sulfuric acid, according to proportioning and concentration, be 10% tosic acid aqueous solution suction hydrolysis kettle (3), ON cycle pump (4), stirs after 30-40 minute, open steam and heat up, in 30-40 minute, be raised to 70-75 ℃; From header tank (1), to hydrolysis kettle (3), add epoxy chloropropane, within 2-3 hour, add, during to control temperature of reaction be 86-93 ℃, react complete, be warming up to 94-102 ℃ and continue reaction 2-3 hour;
Chemical equation is:
Main reaction
Side reaction
Epoxy chlorine alkane hydrin;
B, use recycle pump (4) that hydrolyzed solution is squeezed into hydrolyzed solution header tank (5) after completion of the reaction, then put into ion exchange column (6) and carry out ion-exchange;
First hydrolysis kettle (3) is cooled to 30-40 ℃, then uses recycle pump (4) that hydrolyzed solution is squeezed into hydrolyzed solution header tank (5), then put into ion exchange column (6), adjusting rate of discharge is 0.3-0.4m 3/ h;
C, the ion exchange liquid being comprised of water, glycerin chlorohydrin is added to still kettle (7), open and stir, open steam and heat up, then open waterpower ejector vacuum pump;
First ion exchange liquid is added to still kettle (7), open and stir, open steam and heat up; First boil off moisture, before 101 ℃ of gas phase temperatures, phlegma returns hydrolysis kettle (3) as moisture and continues to use;
When gas phase temperature surpasses 101 ℃, open waterpower ejector vacuum pump, control vacuum tightness is 0.094-0.096MPa;
D, when observing condenser (8) and occur depending on cup dripless to receiving tank, close hydrojet vacuum pump, open successively Roots vacuum system; Mass transport, to front-end volatiles tank (10), and is switched to finished pot (9) by front-end volatiles tank (10);
When observing condenser (8) and occur depending on cup dripless to receiving tank, close hydrojet vacuum pump, open successively Roots vacuum system; Gas phase temperature is front-end volatiles lower than the phlegma of 90 ℃, when gas phase temperature surpasses 0.099MPa since 90 ℃ of in rising trend, system vacuum degree, material is switched to finished pot (9) by front-end volatiles tank (10).
CN201310323361.5A 2013-07-30 2013-07-30 Chloropropanediol purifying apparatus and production method thereof Active CN103360213B (en)

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CN104892365B (en) * 2015-05-27 2017-06-27 泰山医学院 A kind of method of LP synthesizing high-purity glycerin chlorohydrin
CN105626480B (en) * 2015-12-24 2017-12-22 浙江杭真能源科技股份有限公司 The vacuum system of grease device

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Publication number Priority date Publication date Assignee Title
CN102229523A (en) * 2011-05-25 2011-11-02 张中法 Preparation method of 3-chloro-1,2-propanediol
CN102766444A (en) * 2012-08-02 2012-11-07 中国石油化工股份有限公司 Drilling fluid inhibitor and preparation method thereof
CN102786561A (en) * 2012-08-02 2012-11-21 中国石油化工股份有限公司 Method of preparing CAPG for drilling fluid

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102229523A (en) * 2011-05-25 2011-11-02 张中法 Preparation method of 3-chloro-1,2-propanediol
CN102766444A (en) * 2012-08-02 2012-11-07 中国石油化工股份有限公司 Drilling fluid inhibitor and preparation method thereof
CN102786561A (en) * 2012-08-02 2012-11-21 中国石油化工股份有限公司 Method of preparing CAPG for drilling fluid

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