CN105418426A - Device and method for synthesizing cyclohexyl salicylate by adopting solid alkali as catalyst - Google Patents
Device and method for synthesizing cyclohexyl salicylate by adopting solid alkali as catalyst Download PDFInfo
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- CN105418426A CN105418426A CN201510943872.6A CN201510943872A CN105418426A CN 105418426 A CN105418426 A CN 105418426A CN 201510943872 A CN201510943872 A CN 201510943872A CN 105418426 A CN105418426 A CN 105418426A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/03—Preparation of carboxylic acid esters by reacting an ester group with a hydroxy group
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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Abstract
The invention provides a device for synthesizing cyclohexyl salicylate by adopting a solid alkali as a catalyst. The device comprises a cyclohexanol storage tank, a chemical engineering material pump, a cyclohexanol elevated tank, a methyl salicylate elevated tank, an esterification reaction kettle, a fractionating tower A, a spiral plate heat exchanger A, a methanol receiving tank, an automatic back-washing precise filter and a corrosion-resistant material pump, wherein the esterification reaction kettle is in pipe connection with the automatic back-washing precise filter; the automatic back-washing precise filter is in pipe connection with the cyclohexanol elevated tank, and further in pipe connection with a crude reaction product intermediate tank; the crude reaction product intermediate tank is in pipe connection with a water washing kettle and a standing elevated tank; the standing elevated tank is in pipe connection with a kettle-type rectifying tower; the kettle-type rectifying tower is connected with a vacuum receiving tank through a fractionating tower B and a spiral plate heat exchanger B; the vacuum receiving tank is in pipe connection with a product temporary storage tank. The invention further provides a method for producing cyclohexyl salicylate. The device and the method are simple in technology, high in reaction conversion rate, and low in emission of three wastes, and have the advantage that the production cost can be effectively reduced.
Description
Technical field
The present invention relates to technical field of fine chemical synthesis, being specifically related to a kind of take solid alkali as the device of catalyzer salicylate cyclohexyl, present invention also offers the method using above device salicylate cyclohexyl.
Background technology
Whitfield's ointment cyclohexyl has another name called salicylic acid cyclohexyl, C13H16O3, CyclohexylSalicylate, outward appearance is colourless to pale yellow transparent oily liquids, boiling point 115 DEG C/4Pa, flash-point 155 DEG C, relative density 1.112(25/25 DEG C), refractive index 1.532 ~ 1.536(20 DEG C).Have the fragrance of the fragrance of a flower and face cream, fragrance is lasting.Whitfield's ointment cyclohexyl can be used as floral type daily chemical essence formula, and can be used for the floral type daily essences such as allotment yulan, Tuberose, chypre, cape jasmine, jasmine, consumption is within 15%, and IFRA does not limit regulation.In daily chemical essence, be widely used in the raw material as soap use, synthetic detergent and cosmetic essence, especially arrange in pairs or groups with orchidae, n-Hexyl salicylate after using, very effective modified effect can be played to bouquet type composition.Product typical amounts 2-5%, but do not get rid of content in special soap and can reach 10%.
Whitfield's ointment cyclohexyl commercial synthesis is greatly mainly with under the catalyst action such as the vitriol oil, solid acid, Whitfield's ointment and hexalin carry out esterification and obtain crude product, Whitfield's ointment cyclohexyl is obtained through neutralization, washing, vacuum fractionation, the method esterification yield is lower, poor product quality, concentrated acid is very serious to the corrosion of equipment simultaneously, subsequent treatment process is complicated, a large amount of waste water produces environment and pollutes, and, Whitfield's ointment heats at ambient pressure and is easily decomposed into phenol and carbonic acid gas, and the existence of phenol causes the degradation of product aroma quality.Also have and use sodium pyrosulfate as catalyzer, but by product hexyl ether produces in a large number, simultaneous reactions temperature requirement is high, easily causes charing, and product colour is turned black, and follow-up desolventing technology is very difficult.
Summary of the invention
It take solid alkali as the device of catalyzer salicylate cyclohexyl that technical problem to be solved by this invention is to provide a kind of, and its production technique is simple, and reaction conversion ratio is high, and three wastes discharge amount is few, effectively can reduce production cost.
For solving the problems of the technologies described above, of the present invention take solid alkali as the device of catalyzer salicylate cyclohexyl, comprise hexalin storage tank, it is characterized in that: also comprise chemical material pump, hexalin header tank, wintergreen oil header tank, reaction kettle of the esterification, separation column A, spiral-plate heat exchanger A, methyl alcohol receiving tank, automatic back-cleaning precision filter, anticorrosion product pump;
Described hexalin storage tank is connected with hexalin header tank pipeline through chemical material pump, and described hexalin header tank, wintergreen oil header tank are connected with reaction kettle of the esterification pipeline; The hand hole described reaction kettle of the esterification being provided with reactor agitator and feeding intake for catalyzer; Described reaction kettle of the esterification is connected with described separation column A pipeline, and described separation column A is connected with methyl alcohol receiving tank pipeline through spiral-plate heat exchanger A; Described reaction kettle of the esterification is connected with automatic back-cleaning precision filter pipeline; Described automatic back-cleaning precision filter is connected with described hexalin header tank pipeline by anticorrosion product pump; Described automatic back-cleaning precision filter is also connected with crude reaction tundish by pipeline, and described crude reaction tundish are provided with recoil nitrogen inlet; Described crude reaction tundish are connected with washing kettle through pipeline, and described washing kettle is connected with standing header tank through material shifting pump pipeline; Described standing header tank is connected with autoclave rectifying tower by pipeline; Described autoclave rectifying tower is connected with vacuum receiving tank through separation column B and spiral-plate heat exchanger B; Described vacuum receiving tank is connected with product temporary storage tank by pipeline.
Described reaction kettle of the esterification inner side-wall is provided with U-bend, and described automatic back-cleaning precision filter is connected with reaction kettle of the esterification pipeline by U-bend.
Described hexalin storage tank and hexalin header tank outer wall are all provided with lagging facility, and the outer wall of the pipeline between described hexalin storage tank and hexalin header tank, the pipeline between hexalin header tank and reaction kettle of the esterification is all provided with thermal insulation layer.
Silk screen filter core is filled with in described automatic back-cleaning precision filter.
Described autoclave rectifying tower is filled with CY700 filler.
Present invention also offers the method using above device salicylate cyclohexyl, comprise the following steps:
A, hexalin to be squeezed into the hexalin header tank of insulation for subsequent use from the hexalin storage tank of insulation through chemical material pump;
B, in reaction kettle of the esterification, add hexalin from hexalin header tank, in reaction kettle of the esterification, wintergreen oil is added from wintergreen oil header tank, add load type solid body base catalyst from the hand hole of reaction kettle of the esterification, open reaction kettle of the esterification stirrer and mix;
C, open steam valve reaction kettle of the esterification is heated up, control temperature of reaction 120 ~ 150 DEG C, 4 ~ 12 hours reaction times;
After D, dropping terminate, gas chromatographic detection is carried out in sampling, detects at interval of sampling in 1 hour later, and when wintergreen oil content is less than 1.5%, holding temperature continued reaction after 2 hours, cooling termination reaction;
E, pass into nitrogen to reaction kettle of the esterification, reaction solution nitrogen pressure is delivered to automatic back-cleaning precision filter and filters, strainer liquid phase filtrate is pressed onto crude reaction tundish with nitrogen;
F, reaction solution in crude reaction tundish is transferred in washing kettle, add clear water, after turn on agitator stirs 1 hour, by material returned mode at the bottom of still, the crude reaction material shifting pump after washing is squeezed in standing header tank, stratification 2 hours;
After G, standing end, water layer puts into pail pack by leaving standstill the header tank cone end, reuses when next batch is washed; Oil reservoir is transferred in autoclave rectifying tower, rises still temperature to 50 ~ 90 DEG C, and reclaim remaining by-product carbinol under normal pressure, after Methanol Recovery terminates, rise still temperature to 90 ~ 120 DEG C, open water ejector vacuum pump, under 1 ~ 1.67kPa pressure, total reflux, reclaims excessive hexalin; After the condenser that gained hexalin carries through autoclave rectifying tower and spiral-plate heat exchanger B condensation, put into pail pack by vacuum receiving tank collecting ring hexanol; After hexalin reclaims and terminates, rise still temperature to 120 ~ 180 DEG C, open water ejector vacuum pump+Roots vaccum pump combination vacuum pump set, fractionation is carried out under vacuum pressure 133 ~ 1000Pa, tower top temperature 120 ~ 150 DEG C, reflux ratio 1: 1 ~ 1: 12 condition, after the condenser that gained Whitfield's ointment cyclohexyl carries through autoclave rectifying tower and spiral-plate heat exchanger B condensation, collect Whitfield's ointment cyclohexyl product by vacuum receiving tank 17, put into product temporary storage tank.
In described step B, by separation column A, spiral-plate heat exchanger A, the methyl alcohol of condensation is put into methyl alcohol receiving tank.
In described step e, hexalin is squeezed into through anticorrosion product pump to automatic back-cleaning precision filter from hexalin header tank, and pass into nitrogen by the recoil nitrogen inlet of crude reaction tundish, solid-phase catalyst pressurized backwash on silk screen filter core, in reaction kettle of the esterification, is applied mechanically when directly carrying out lower batch of reaction.
Technological merit of the present invention:
1. provide a set of cleaning production apparatus for the synthesis of Whitfield's ointment cyclohexyl.This device can adopt wintergreen oil and hexalin to be main raw material, and under catalyzed by solid base, carry out transesterification reaction under effect, single stage method prepares Whitfield's ointment cyclohexyl crude product, and after filtration, neutralization &washing, rectifying obtains Whitfield's ointment cyclohexyl finished product.
2, wintergreen oil is adopted to be main raw material salicylate cyclohexyl, overcome with Whitfield's ointment when being main raw material, the generation of side reaction thing phenol, thus prevent the unpleasant odor that it is charred product fragrance generation plastics, ensure that the pure and soft of product fragrance, avoid simultaneously residual in the product very low levels Whitfield's ointment bring final finished color with more rose pink problem, and the peach desolventing technology of product tape is also very difficult.
3. automatic back-cleaning precision filter can realize the automatic filtration back flushing of solid catalyst, overcome the catalyst loss shifted in sedimentation filtration process and the shortcoming being caused catalyst deactivation by outside contamination, there is airtight safety in production, simple to operate, filter operation can be carried out in a long time continuously, filtering accuracy is high, ensure the feature of quality product, reduce the operation of manual switching frequently and heavy cleaning filter work, avoid unnecessary shut-down, thus protect expensive catalyzer, shorten single batch operation cycle of production equipment, reduce production cost.Crude reaction tundish are provided with recoil nitrogen inlet, when needing to reclaim solid catalyst, nitrogen pressure can be utilized to be pressed in reaction kettle of the esterification by solid catalyst.
4. use device provided by the present invention to produce, raw material sources are easy to get, and reaction conditions is gentle, and reaction conversion ratio is high, and technics comparing is easily implemented, and produce three wastes discharge amount in production process few, product yield is greatly improved, and belongs to process for cleanly preparing.
Due to described reaction kettle of the esterification being directly connected with separation column A by pipeline, thus can from reaction system, by-product carbinol be moved in methyl alcohol receiving tank from reactor in time.
Accompanying drawing explanation
The structural representation of Fig. 1 to be of the present invention with solid alkali be device of catalyzer salicylate cyclohexyl.
In figure: 1-hexalin storage tank, 2-chemical material pump, 3-hexalin header tank, 4-wintergreen oil header tank, 5-reaction kettle of the esterification, 51-reactor agitator, 52-U-tube, 53-hand hole, 6-separation column A, 6 '-separation column B, 7-spiral-plate heat exchanger A, 8-methyl alcohol receiving tank, 9-automatic back-cleaning precision filter, 91-silk screen filter core, 10-anticorrosion product pump, 11-crude reaction tundish, 111-recoil nitrogen inlet, 12-washing kettle, 13-material shifting pump, 14-leave standstill header tank, 15-autoclave rectifying tower, 16-spiral-plate heat exchanger B, 17-vacuum receiving tank, 18-product temporary storage tank.
Embodiment
As shown in Figure 1, of the present invention take solid alkali as the device of catalyzer salicylate cyclohexyl, comprise hexalin storage tank 1, also comprise chemical material pump 2, hexalin header tank 3, wintergreen oil header tank 4, reaction kettle of the esterification 5, separation column A6, spiral-plate heat exchanger A7, methyl alcohol receiving tank 8, automatic back-cleaning precision filter 9, anticorrosion product pump 10; Described hexalin storage tank 1 is connected with hexalin header tank 3 pipeline through chemical material pump 2, and described hexalin header tank 3, wintergreen oil header tank 4 are connected with reaction kettle of the esterification 5 pipeline; The hand hole 53 described reaction kettle of the esterification 5 being provided with reactor agitator 51 and feeding intake for catalyzer; Described reaction kettle of the esterification 5 is connected with described separation column A6 pipeline, and described separation column A6 is connected with methyl alcohol receiving tank 8 pipeline through spiral-plate heat exchanger A7; Described reaction kettle of the esterification 5 is connected with automatic back-cleaning precision filter 9 pipeline; Described automatic back-cleaning precision filter 9 is connected with described hexalin header tank 3 pipeline by anticorrosion product pump 10; Described automatic back-cleaning precision filter 9 is also connected with crude reaction tundish 11 by pipeline, described crude reaction tundish 11 is provided with recoil nitrogen inlet 111; Described crude reaction tundish 11 are connected with washing kettle 12 through pipeline, and described washing kettle 12 is connected with standing header tank 14 through material shifting pump 13 pipeline; Described standing header tank 14 is connected with autoclave rectifying tower 15 by pipeline; Described autoclave rectifying tower 15 is connected with vacuum receiving tank 17 through separation column B6 ' and spiral-plate heat exchanger B16; Described vacuum receiving tank 17 is connected with product temporary storage tank 18 by pipeline.
Described hexalin storage tank 1 is all provided with lagging facility with hexalin header tank 3 outer wall, and the outer wall of the pipeline between described hexalin storage tank 1 and hexalin header tank 3, the pipeline between hexalin header tank 3 and reaction kettle of the esterification 5 is all provided with thermal insulation layer.
Silk screen filter core 91 is filled with in described automatic back-cleaning precision filter 9.
The concrete steps using the present invention to produce Whitfield's ointment cyclohexyl comprise:
Hexalin to be squeezed into the hexalin header tank 3 of insulation for subsequent use from the hexalin storage tank 1 of insulation through chemical material pump 2.
In reaction kettle of the esterification 5, add hexalin, wintergreen oil from hexalin header tank 3, wintergreen oil header tank 4, add load type solid body base catalyst from reaction kettle of the esterification 5 hand hole 53, open reactor agitator 51 and mix.
Described reaction kettle of the esterification 5 is 50L ~ 5000L enamel reaction still, and described reaction kettle of the esterification 5 upper end is connected with separation column A6 by pipeline, and for separating the by-product carbinol produced by reaction in reaction system in time, the forward being beneficial to react carries out.
Described separation column A6 is connected with spiral-plate heat exchanger A7 by pipeline, and the methyl alcohol of condensation is put into methyl alcohol receiving tank 8.
Connecting tube between described hexalin header tank 3 and reaction kettle of the esterification 5 should install attemperator additional.
Open steam valve to heat up to reaction kettle of the esterification 5, control temperature of reaction 120 ~ 150 DEG C, 4 ~ 12 hours reaction times.
After dropping terminates, gas chromatographic detection is carried out in sampling, detects at interval of sampling in 1 hour later, and when wintergreen oil content is less than 1.5%, holding temperature continued reaction after 2 hours, cooling termination reaction.
Described reaction kettle of the esterification 5 inner side-wall is provided with U-bend 52, and automatic back-cleaning precision filter 9 is connected with reaction kettle of the esterification 5 by U-bend 52.Nitrogen is passed into reaction kettle of the esterification 5, reaction solution nitrogen pressure is delivered to automatic back-cleaning precision filter 9 filter, after strainer liquid phase filtrate is pressed onto crude reaction tundish 11 with nitrogen, solid-phase catalyst for filtering on silk screen filter core 91 can be taked with under type process: squeeze into hexalin through anticorrosion product pump 10 to automatic back-cleaning precision filter 9 from hexalin header tank 3, and pass into nitrogen by the recoil nitrogen inlet 111 of crude reaction tundish 11, thus by solid-phase catalyst pressurized backwash in reaction kettle of the esterification 5, apply mechanically when directly carrying out lower batch of reaction.
Reaction solution in crude reaction tundish 11 is transferred in washing kettle 12, adds clear water, after turn on agitator stirs 1 hour, by material returned mode at the bottom of still, the crude reaction material shifting pump 13 after washing is squeezed in standing header tank 14, stratification 2 hours.
Leave standstill after terminating, water layer puts into pail pack by leaving standstill the header tank cone end, reuses when next batch is washed.Oil reservoir is transferred in autoclave rectifying tower 15 by high potential difference, rises still temperature to 50 ~ 90 DEG C, reclaims remaining by-product carbinol under normal pressure, after Methanol Recovery terminates, rise still temperature to 90 ~ 120 DEG C, open water ejector vacuum pump, under 1 ~ 1.67kPa pressure, total reflux, reclaims excessive hexalin; After the condenser that gained hexalin carries through autoclave rectifying tower 15 and spiral-plate heat exchanger B6 ' condensation, put into pail pack by vacuum receiving tank 17 collecting ring hexanol.After hexalin reclaims and terminates, rise still temperature to 120 ~ 180 DEG C, open water ejector vacuum pump+Roots vaccum pump combination vacuum pump set, fractionation is carried out under vacuum pressure 133 ~ 1000Pa, tower top temperature 120 ~ 150 DEG C, reflux ratio 1: 1 ~ 1: 12 condition, after the condenser that gained Whitfield's ointment cyclohexyl carries through autoclave rectifying tower 15 and spiral-plate heat exchanger B6 ' condensation, collected the Whitfield's ointment cyclohexyl product obtaining content 99% by vacuum receiving tank 17, put into product temporary storage tank 18.
Described autoclave rectifying tower 15 loads as CY700 type filler.
Made product is colourless transparent liquid, has the fragrance of the fragrance of a flower and face cream, is 99.36% through gas chromatographic analysis product purity, and detecting refractive index (20 DEG C) is 1.5336, and relative density (25 DEG C) is 1.1124, and phenol content does not detect.
Technique scheme adopts wintergreen oil and hexalin to be main raw material, and under catalyzed by solid base, carry out transesterification reaction under effect, single stage method prepares Whitfield's ointment cyclohexyl crude product, and after filtration, neutralization &washing, rectifying obtains Whitfield's ointment cyclohexyl finished product.Wintergreen oil is adopted to be main raw material salicylate cyclohexyl, overcome with Whitfield's ointment when being main raw material, the generation of side reaction phenol, prevent the unpleasant odor that product fragrance generation plastics are charred, ensure that the pure and soft of product fragrance, avoid simultaneously residual in the product very low levels Whitfield's ointment bring final finished color with more rose pink problem, and the peach desolventing technology of product tape is also very difficult.
Back flushing after solid catalyst automatic filtration; overcome the catalyst loss shifted in sedimentation filtration process and the shortcoming being caused catalyst deactivation by outside contamination; there is airtight safety in production, simple to operate, the feature that makes that filter operation can be carried out in a long time continuously, filtering accuracy is high, ensure quality product; reduce the operation of manual switching frequently and heavy cleaning filter work; avoid unnecessary shut-down; thus protect expensive catalyzer; shorten single batch operation cycle of production equipment, reduce production cost.This method raw material sources are easy to get, and reaction conditions is gentle, and reaction conversion ratio is high, and technics comparing is easily implemented, and produce three wastes discharge amount in production process few, product yield is greatly improved, and belongs to process for cleanly preparing.
Claims (8)
1. one kind take solid alkali as the device of catalyzer salicylate cyclohexyl, comprise hexalin storage tank (1), it is characterized in that: also comprise chemical material pump (2), hexalin header tank (3), wintergreen oil header tank (4), reaction kettle of the esterification (5), separation column A(6), spiral-plate heat exchanger A(7), methyl alcohol receiving tank (8), automatic back-cleaning precision filter (9), anticorrosion product pump (10);
Described hexalin storage tank (1) is connected with hexalin header tank (3) pipeline through chemical material pump (2), and described hexalin header tank (3), wintergreen oil header tank (4) are connected with reaction kettle of the esterification (5) pipeline; The hand hole (53) described reaction kettle of the esterification (5) being provided with reactor agitator (51) and feeding intake for catalyzer; Described reaction kettle of the esterification (5) and described separation column A(6) pipeline is connected, described separation column A(6) through spiral-plate heat exchanger A(7) be connected with methyl alcohol receiving tank (8) pipeline; Described reaction kettle of the esterification (5) is connected with automatic back-cleaning precision filter (9) pipeline; Described automatic back-cleaning precision filter (9) is connected with described hexalin header tank (3) pipeline by described anticorrosion product pump (10); Described automatic back-cleaning precision filter (9) is also connected with crude reaction tundish (11) by pipeline, described crude reaction tundish (11) is provided with recoil nitrogen inlet (111); Described crude reaction tundish (11) are connected with washing kettle (12) through pipeline, and described washing kettle (12) is connected with standing header tank (14) through material shifting pump (13) pipeline; Described standing header tank (14) is connected with autoclave rectifying tower (15) by pipeline; Described autoclave rectifying tower (15) is through separation column B(6 ') and spiral-plate heat exchanger B(16) be connected with vacuum receiving tank (17); Described vacuum receiving tank (17) is connected with product temporary storage tank (18) by pipeline.
2. be the device of catalyzer salicylate cyclohexyl as claimed in claim 1 with solid alkali, it is characterized in that: described reaction kettle of the esterification (5) inner side-wall is provided with U-bend (52), described automatic back-cleaning precision filter (9) is connected with reaction kettle of the esterification (5) pipeline by U-bend (52).
3. be the device of catalyzer salicylate cyclohexyl as claimed in claim 1 or 2 with solid alkali, it is characterized in that: described hexalin storage tank (1) and hexalin header tank (3) outer wall are all provided with lagging facility, and the outer wall of the pipeline between described hexalin storage tank (1) and hexalin header tank (3), the pipeline between hexalin header tank (3) and reaction kettle of the esterification (5) is all provided with thermal insulation layer.
4. be the device of catalyzer salicylate cyclohexyl as claimed in claim 3 with solid alkali, it is characterized in that: in described automatic back-cleaning precision filter (9), be filled with silk screen filter core (91).
5. be the device of catalyzer salicylate cyclohexyl as claimed in claim 4 with solid alkali, it is characterized in that: described autoclave rectifying tower (15) is filled with CY700 filler.
6. use the method for the device salicylate cyclohexyl described in claim 5, comprise the following steps:
A, hexalin to be squeezed into the hexalin header tank (3) of insulation for subsequent use from the hexalin storage tank (1) of insulation through chemical material pump (2);
B, in reaction kettle of the esterification (5), add hexalin from hexalin header tank (3), in reaction kettle of the esterification (5), wintergreen oil is added from wintergreen oil header tank (4), add load type solid body base catalyst from the hand hole (53) of reaction kettle of the esterification (5), open reaction kettle of the esterification stirrer (51) and mix;
C, open steam valve reaction kettle of the esterification (5) is heated up, control temperature of reaction 120 ~ 150 DEG C, 4 ~ 12 hours reaction times;
After D, dropping terminate, gas chromatographic detection is carried out in sampling, detects at interval of sampling in 1 hour later, and when wintergreen oil content is less than 1.5%, holding temperature continued reaction after 2 hours, cooling termination reaction;
E, pass into nitrogen to reaction kettle of the esterification (5), reaction solution nitrogen pressure is delivered to automatic back-cleaning precision filter (9) and filter, strainer liquid phase filtrate is pressed onto crude reaction tundish (11) with nitrogen;
F, crude reaction tundish (11) interior reaction solution is transferred in washing kettle (12), add clear water, after turn on agitator stirs 1 hour, by material returned mode at the bottom of still, the crude reaction material shifting pump (13) after washing is squeezed in standing header tank (14), stratification 2 hours;
After G, standing end, water layer puts into pail pack by leaving standstill header tank (14) the cone end, reuses when next batch is washed; Oil reservoir is transferred in autoclave rectifying tower (15), rises still temperature to 50 ~ 90 DEG C, reclaims remaining by-product carbinol under normal pressure, after Methanol Recovery terminates, rise still temperature to 90 ~ 120 DEG C, open water ejector vacuum pump, under 1 ~ 1.67kPa pressure, total reflux, reclaims excessive hexalin; The condenser that gained hexalin carries through autoclave rectifying tower (15) and spiral-plate heat exchanger B(6 ') after condensation, put into pail pack by vacuum receiving tank (17) collecting ring hexanol; After hexalin reclaims and terminates, rise still temperature to 120 ~ 180 DEG C, open water ejector vacuum pump+Roots vaccum pump combination vacuum pump set, fractionation is carried out under vacuum pressure 133 ~ 1000Pa, tower top temperature 120 ~ 150 DEG C, reflux ratio 1: 1 ~ 1: 12 condition, the condenser that gained Whitfield's ointment cyclohexyl carries through autoclave rectifying tower (15) and spiral-plate heat exchanger B(6 ') after condensation, collect Whitfield's ointment cyclohexyl product by vacuum receiving tank 17, put into product temporary storage tank (18).
7. the method for salicylate cyclohexyl as claimed in claim 6, is characterized in that: in described step B, by separation column A(6), spiral-plate heat exchanger A(7), the methyl alcohol of condensation is put into methyl alcohol receiving tank (8).
8. the method for salicylate cyclohexyl as claimed in claim 6, it is characterized in that: described step e also comprises, hexalin is squeezed into through anticorrosion product pump (10) to automatic back-cleaning precision filter (9) from hexalin header tank (3), and pass into nitrogen by the recoil nitrogen inlet (111) of crude reaction tundish (11), solid-phase catalyst pressurized backwash on silk screen filter core (91), in reaction kettle of the esterification (5), is applied mechanically when directly carrying out lower batch of reaction.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510943872.6A CN105418426A (en) | 2015-12-17 | 2015-12-17 | Device and method for synthesizing cyclohexyl salicylate by adopting solid alkali as catalyst |
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| CN201510943872.6A CN105418426A (en) | 2015-12-17 | 2015-12-17 | Device and method for synthesizing cyclohexyl salicylate by adopting solid alkali as catalyst |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106674009A (en) * | 2017-03-17 | 2017-05-17 | 濮阳市盛源能源科技股份有限公司 | Reaction device for synthetic production of diisooctyl sebacate, and synthetic process method of diisooctyl sebacate |
| CN111423317A (en) * | 2020-03-12 | 2020-07-17 | 安徽华业香料股份有限公司 | Production device and method for synthesizing dihydro jasmone spice through solid acid catalysis |
| CN112592278A (en) * | 2020-12-25 | 2021-04-02 | 安徽华业香料股份有限公司 | Production device and method for synthesizing musk xylol from propiolactone by-product |
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2015
- 2015-12-17 CN CN201510943872.6A patent/CN105418426A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106674009A (en) * | 2017-03-17 | 2017-05-17 | 濮阳市盛源能源科技股份有限公司 | Reaction device for synthetic production of diisooctyl sebacate, and synthetic process method of diisooctyl sebacate |
| CN111423317A (en) * | 2020-03-12 | 2020-07-17 | 安徽华业香料股份有限公司 | Production device and method for synthesizing dihydro jasmone spice through solid acid catalysis |
| CN111423317B (en) * | 2020-03-12 | 2022-11-22 | 安徽华业香料股份有限公司 | Production device and method for synthesizing dihydro jasmone spice through solid acid catalysis |
| CN112592278A (en) * | 2020-12-25 | 2021-04-02 | 安徽华业香料股份有限公司 | Production device and method for synthesizing musk xylol from propiolactone by-product |
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