CN205241572U - Use device of solid base as own ester of synthetic salicylic acid ring of catalyst - Google Patents
Use device of solid base as own ester of synthetic salicylic acid ring of catalyst Download PDFInfo
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- CN205241572U CN205241572U CN201521052615.5U CN201521052615U CN205241572U CN 205241572 U CN205241572 U CN 205241572U CN 201521052615 U CN201521052615 U CN 201521052615U CN 205241572 U CN205241572 U CN 205241572U
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Abstract
The utility model provides an use device of solid base as own ester of synthetic salicylic acid ring of catalyst, receive jar, automatic back flush precision filter, anticorrosive material pump including cyclohexanol storage tank, chemical material pump, cyclohexanol elevated tank, methyl salicylate elevated tank, esterification reaction cauldron, fractionating tower A, spiral plate heat exchanger A, methyl alcohol, esterification reaction cauldron and automatic back flush precision filter pipe connection, automatic back flush precision filter and cyclohexanol elevated tank pipe connection, still respond the crude pans through the pipe connection, reaction crude pans manage say be connected with water washing kettle, the elevated tank stews, the elevated tank that stews there is cauldron formula rectifying column through the pipe connection, cauldron formula rectifying column is connected with vacuum receipt jar through fractionating tower B and spiral plate heat exchanger B, receive jar in the vacuum has the product jar of keeping in through the pipe connection. The utility model discloses still provide its production method, its simple process, conversion are rateed highly, and three wastes emission is few, effectively reduction in production cost.
Description
Technical field
The utility model relates to technical field of fine chemical synthesis, is specifically related to a kind of device taking solid base as catalyst salicylate cyclohexyl.
Background technology
Salicylic acid cyclohexyl has another name called salicylic acid cyclohexyl, C13H16O3, CyclohexylSalicylate, outward appearance is colourless to faint yellow transparent oily liquid, 115 DEG C/4Pa of boiling point, 155 DEG C of flash-points, relative density 1.112(25/25 DEG C), refraction index 1.532 ~ 1.536(20 DEG C). The fragrance with the fragrance of a flower and face cream, fragrance is lasting. Salicylic acid cyclohexyl can be used as floral type daily chemical essence formula, can be used for allocating the floral type daily essences such as yulan, tuberose, chypre, cape jasmine, jasmine, and consumption is in 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, after especially using with amyl salicylate, 1-Hexyl salicylate collocation, can play very effectively modified effect to bouquet type composition. Product typical amounts 2-5%, can reach 10% but do not get rid of content in special soap.
The industry of salicylic acid cyclohexyl is synthetic greatly mainly with under the catalyst action such as the concentrated sulfuric acid, solid acid, salicylic acid and cyclohexanol carry out esterification and obtain crude product, make salicylic acid cyclohexyl 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 complexity, a large amount of waste water produces and pollutes environment, and, salicylic acid heats and is easily decomposed into phenol and carbon dioxide under normal pressure, and the existence of phenol causes the degradation of product aroma quality. Also have the niter cake of use as catalyst, but accessory substance hexyl ether produces in a large number, simultaneous reactions temperature requirement is high, easily causes charing, makes product colour blackout, and follow-up decolouring is processed very difficult.
Summary of the invention
Technical problem to be solved in the utility model is to provide a kind of device taking solid base as catalyst salicylate cyclohexyl, and its production technology is simple, and reaction conversion ratio is high, and three wastes discharge amount is few, can effectively reduce production costs.
For solving the problems of the technologies described above, device taking solid base as catalyst salicylate cyclohexyl of the present utility model, comprise cyclohexanol storage tank, it is characterized in that: also comprise chemical material pump, cyclohexanol head tank, gaultherolin head tank, reaction kettle of the esterification, fractionating column A, spiral-plate heat exchanger A, methyl alcohol receiving tank, automatic back-cleaning precision filter, anticorrosion product pump;
Described cyclohexanol storage tank is connected with cyclohexanol head tank pipeline through chemical material pump, and described cyclohexanol head tank, gaultherolin head tank are connected with reaction kettle of the esterification pipeline; The hand hole that is provided with reactor agitator on described reaction kettle of the esterification and feeds intake for catalyst; Described reaction kettle of the esterification is connected with described fractionating column A pipeline, and described fractionating 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 cyclohexanol head tank pipeline by anticorrosion product pump; Described automatic back-cleaning precision filter is also connected with crude reaction pans by pipeline, on described crude reaction pans, is provided with recoil nitrogen inlet; Described crude reaction pans are connected with washing kettle through pipeline, and described washing kettle is connected with standing head tank through material shifting pump pipeline; Described standing head tank is connected with autoclave rectifying column by pipeline; Described autoclave rectifying column is connected with vacuum receiving tank through fractionating column B and spiral-plate heat exchanger B; Described vacuum receiving tank is connected with the temporary tank of product by pipeline.
On described reaction kettle of the esterification madial wall, be provided with U-bend, described automatic back-cleaning precision filter is connected with reaction kettle of the esterification pipeline by U-bend.
Described cyclohexanol storage tank and cyclohexanol head tank outer wall are all provided with lagging facility, on the outer wall of the pipeline between pipeline, cyclohexanol head tank and reaction kettle of the esterification between described cyclohexanol storage tank and cyclohexanol head tank, are all provided with heat-insulation layer.
In described automatic back-cleaning precision filter, be filled with silk screen filter core.
Described autoclave rectifying column is filled with CY700 filler.
The utility model also provides the method that uses above device salicylate cyclohexyl, comprises the following steps:
A, cyclohexanol is squeezed into the cyclohexanol head tank of insulation for subsequent use from the cyclohexanol storage tank of insulation through chemical material pump;
B, add cyclohexanol in from cyclohexanol head tank to reaction kettle of the esterification, in from gaultherolin head tank to reaction kettle of the esterification, add gaultherolin, add load type solid body base catalyst from the hand hole of reaction kettle of the esterification, open reaction kettle of the esterification mixer and mix;
C, open steam valve reaction kettle of the esterification is heated up, control 120 ~ 150 DEG C of reaction temperatures, 4 ~ 12 hours reaction time;
After D, dropping finish, gas chromatographic detection is carried out in sampling, detects at interval of sampling in 1 hour later, and in the time that gaultherolin content is less than 1.5%, holding temperature continued reaction after 2 hours, the cessation reaction of lowering the temperature;
E, pass into nitrogen to reaction kettle of the esterification, reactant liquor is delivered to automatic back-cleaning precision filter by nitrogen pressure and filter, filter liquid phase filtrate is pressed onto crude reaction pans with nitrogen;
F, reactant liquor in crude reaction pans is transferred in washing kettle, added clear water, turn on agitator stirred after 1 hour, by material returned mode at the bottom of still, the crude reaction after washing was squeezed in standing head tank to stratification 2 hours with material shifting pump;
After G, standing end, water layer is put into pail pack, recycling in the time that next batch is washed by leaving standstill the head tank cone end; Oil reservoir is transferred in autoclave rectifying column, rises still temperature to 50 ~ 90 DEG C, reclaims remaining by-product carbinol under normal pressure, after Methanol Recovery finishes, rises still temperature to 90 ~ 120 DEG C, open water ejector vacuum pump, and under 1 ~ 1.67kPa pressure, infinite reflux, reclaims excessive cyclohexanol; After the condenser that gained cyclohexanol carries through autoclave rectifying column and spiral-plate heat exchanger B condensation, put into pail pack by vacuum receiving tank collecting ring hexanol; After cyclohexanol reclaims and finishes, rise still temperature to 120 ~ 180 DEG C, open water ejector vacuum pump+Roots vaccum pump combination vacuum unit, within 1: 1～1: 12, under condition, carry out fractionation in vacuum pressure 133～1000Pa, 120～150 DEG C of tower top temperatures, reflux ratio, after the condenser that gained salicylic acid cyclohexyl carries through autoclave rectifying column and spiral-plate heat exchanger B condensation, collect salicylic acid cyclohexyl product by vacuum receiving tank 17, put into the temporary tank of product.
In described step B, by fractionating column A, spiral-plate heat exchanger A, the methyl alcohol of condensation is put into methyl alcohol receiving tank.
In described step e, squeeze into cyclohexanol through anticorrosion product pump to automatic back-cleaning precision filter from cyclohexanol head tank, and pass into nitrogen by the recoil nitrogen inlet of crude reaction pans, solid-phase catalyst pressurized backwash on silk screen filter core, to reaction kettle of the esterification, is applied mechanically while directly carrying out lower batch of reaction.
Technological merit of the present utility model:
1. provide a set of for the synthetic cleaning production apparatus of salicylic acid cyclohexyl. It is primary raw material that this device can adopt gaultherolin and cyclohexanol, under catalyzed by solid base, under effect, carries out ester exchange reaction, and one-step method is prepared salicylic acid cyclohexyl crude product, after filtration, neutralization washing, rectifying obtain salicylic acid cyclohexyl finished product.
2, adopting gaultherolin is primary raw material salicylate cyclohexyl, while having overcome taking salicylic acid as primary raw material, the generation of side reaction thing phenol, thereby prevent that it from producing to product fragrance the bad smell that plastics are charred, ensure the pure and soft of product fragrance, avoided remaining in product the very salicylic acid of low content simultaneously and brought final finished color with more rose pink problem, and the peach decolouring of product tape is processed also very difficult.
3. automatic back-cleaning precision filter can be realized the automatic fitration backwash of solid catalyst, overcome the shortcoming that shifts the catalyst loss in sedimentation filter process and caused catalysqt 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 product quality, reduce the operation of manual switching frequently and heavy cleaning filter work, avoid unnecessary shut-down, thereby protect expensive catalyst, shorten single batch operation cycle of process units, reduce production costs. on crude reaction pans, be provided with recoil nitrogen inlet, need to reclaim solid catalyst time, can utilize nitrogen pressure that solid catalyst is pressed in reaction kettle of the esterification.
4. use device provided by the utility model to produce, raw material sources are easy to get, reaction condition gentleness, and reaction conversion ratio is high, and technique ratio is easier to implement, and produces three wastes discharge amount few in production process, and product yield is greatly improved, and belongs to process for cleanly preparing.
Owing to being directly connected with fractionating column A by pipeline on described reaction kettle of the esterification, thereby can from reaction system, by-product carbinol be moved in methyl alcohol receiving tank from reactor in time.
Brief description of the drawings
Fig. 1 is the structural representation taking solid base as the device of catalyst salicylate cyclohexyl of the present utility model.
In figure: 1-cyclohexanol storage tank, 2-chemical material pump, 3-cyclohexanol head tank, 4-gaultherolin head tank, 5-reaction kettle of the esterification, 51-reactor agitator, 52-U-shaped pipe, 53-hand hole, 6-fractionating column A, 6 '-fractionating 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 pans, 111-recoil nitrogen inlet, 12-washing kettle, 13-material shifting pump, 14-standing head tank, 15-autoclave rectifying column, 16-spiral-plate heat exchanger B, 17-vacuum receiving tank, 18-product is kept in tank.
Detailed description of the invention
As shown in Figure 1, device taking solid base as catalyst salicylate cyclohexyl of the present utility model, comprise cyclohexanol storage tank 1, also comprise chemical material pump 2, cyclohexanol head tank 3, gaultherolin head tank 4, reaction kettle of the esterification 5, fractionating column A6, spiral-plate heat exchanger A7, methyl alcohol receiving tank 8, automatic back-cleaning precision filter 9, anticorrosion product pump 10; Described cyclohexanol storage tank 1 is connected with cyclohexanol head tank 3 pipelines through chemical material pump 2, and described cyclohexanol head tank 3, gaultherolin head tank 4 are connected with reaction kettle of the esterification 5 pipelines; The hand hole 53 that is provided with reactor agitator 51 and feeds intake for catalyst on described reaction kettle of the esterification 5; Described reaction kettle of the esterification 5 is connected with described fractionating column A6 pipeline, and described fractionating column A6 is connected with methyl alcohol receiving tank 8 pipelines through spiral-plate heat exchanger A7; Described reaction kettle of the esterification 5 is connected with automatic back-cleaning precision filter 9 pipelines; Described automatic back-cleaning precision filter 9 is connected with described cyclohexanol head tank 3 pipelines by anticorrosion product pump 10; Described automatic back-cleaning precision filter 9 is also connected with crude reaction pans 11 by pipeline, is provided with recoil nitrogen inlet 111 on described crude reaction pans 11; Described crude reaction pans 11 are connected with washing kettle 12 through pipeline, and described washing kettle 12 is connected with and leaves standstill head tank 14 through material shifting pump 13 pipelines; Described standing head tank 14 is connected with autoclave rectifying column 15 by pipeline; Described autoclave rectifying column 15 is connected with vacuum receiving tank 17 through fractionating column B6 ' and spiral-plate heat exchanger B16; Described vacuum receiving tank 17 is connected with the temporary tank 18 of product by pipeline.
Described cyclohexanol storage tank 1 is all provided with lagging facility with cyclohexanol head tank 3 outer walls, on the outer wall of the pipeline between pipeline, cyclohexanol head tank 3 and reaction kettle of the esterification 5 between described cyclohexanol storage tank 1 and cyclohexanol head tank 3, is all provided with heat-insulation layer.
In described automatic back-cleaning precision filter 9, be filled with silk screen filter core 91.
The concrete steps that use the utility model to produce salicylic acid cyclohexyl comprise:
Cyclohexanol is squeezed into the cyclohexanol head tank 3 of insulation for subsequent use from the cyclohexanol storage tank 1 of insulation through chemical material pump 2.
In reaction kettle of the esterification 5, add cyclohexanol, gaultherolin from cyclohexanol head tank 3, gaultherolin head tank 4, add load type solid body base catalyst from reaction kettle of the esterification 5 hand holes 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 ends are connected with fractionating column A6 by pipeline, the by-product carbinol being produced by reaction for separating in time reaction system, and the forward that is beneficial to reaction carries out.
Described fractionating 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 pipe between described cyclohexanol head tank 3 and reaction kettle of the esterification 5 should install attemperator additional.
Open steam valve reaction kettle of the esterification 5 is heated up, control 120 ~ 150 DEG C of reaction temperatures, 4 ~ 12 hours reaction time.
After dropping finishes, gas chromatographic detection is carried out in sampling, detects at interval of sampling in 1 hour later, and in the time that gaultherolin content is less than 1.5%, holding temperature continued reaction after 2 hours, cooling cessation reaction.
On described reaction kettle of the esterification 5 madial walls, be provided with U-bend 52, automatic back-cleaning precision filter 9 is connected with reaction kettle of the esterification 5 by U-bend 52. pass into nitrogen to reaction kettle of the esterification 5, reactant liquor is delivered to automatic back-cleaning precision filter 9 by nitrogen pressure to be filtered, filter liquid phase filtrate is pressed onto after crude reaction pans 11 with nitrogen, can take following mode processing for the solid-phase catalyst of filtering on silk screen filter core 91: squeeze into cyclohexanol through anticorrosion product pump 10 to automatic back-cleaning precision filter 9 from cyclohexanol head tank 3, and pass into nitrogen by the recoil nitrogen inlet 111 of crude reaction pans 11, thereby by solid-phase catalyst pressurized backwash to reaction kettle of the esterification 5, while directly carrying out lower batch of reaction, apply mechanically.
Interior crude reaction pans 11 reactant liquor is transferred in washing kettle 12, added clear water, turn on agitator stirred after 1 hour, by material returned mode at the bottom of still, the crude reaction after washing was squeezed into and was left standstill in head tank 14 with material shifting pump 13, stratification 2 hours.
Leave standstill after end, water layer is put into pail pack, recycling in the time that next batch is washed by leaving standstill the head tank cone end. Oil reservoir is transferred in autoclave rectifying column 15 by high potential difference, rises still temperature to 50 ~ 90 DEG C, reclaims remaining by-product carbinol under normal pressure, after Methanol Recovery finishes, rise still temperature to 90 ~ 120 DEG C, open water ejector vacuum pump, under 1 ~ 1.67kPa pressure, infinite reflux, reclaims excessive cyclohexanol; After the condenser that gained cyclohexanol carries through autoclave rectifying column 15 and spiral-plate heat exchanger B6 ' condensation, put into pail pack by vacuum receiving tank 17 collecting ring hexanols. After cyclohexanol reclaims and finishes, rise still temperature to 120 ~ 180 DEG C, open water ejector vacuum pump+Roots vaccum pump combination vacuum unit, within 1: 1～1: 12, under condition, carry out fractionation in vacuum pressure 133～1000Pa, 120～150 DEG C of tower top temperatures, reflux ratio, after the condenser that gained salicylic acid cyclohexyl carries through autoclave rectifying column 15 and spiral-plate heat exchanger B6 ' condensation, collect by vacuum receiving tank 17 the salicylic acid cyclohexyl product that obtains content 99%, put into the temporary tank 18 of product.
Described autoclave rectifying column 15 fillings are 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 refraction index (20 DEG C) is 1.5336, and relative density (25 DEG C) is 1.1124, and phenol content does not detect.
It is primary raw material that technique scheme adopts gaultherolin and cyclohexanol, under catalyzed by solid base, under effect, carries out ester exchange reaction, and one-step method is prepared salicylic acid cyclohexyl crude product, after filtration, neutralization washing, rectifying obtain salicylic acid cyclohexyl finished product. Adopting gaultherolin is primary raw material salicylate cyclohexyl, while having overcome taking salicylic acid as primary raw material, the generation of side reaction phenol, prevent product fragrance to produce the bad smell that plastics are charred, ensure the pure and soft of product fragrance, avoided remaining in product the very salicylic acid of low content simultaneously and brought final finished color with more rose pink problem, and the peach decolouring of product tape is processed also very difficult.
Backwash after solid catalyst automatic fitration; overcome the shortcoming that shifts the catalyst loss in sedimentation filter process and caused catalysqt deactivation by outside contamination; have airtight safety in production, simple to operate, make that filter operation can be carried out in a long time continuously, filtering accuracy is high, ensure the feature of product quality; reduce the operation of manual switching frequently and heavy cleaning filter work; avoid unnecessary shut-down; thereby protect expensive catalyst; in the single batch operation cycle that has shortened process units, reduce production costs. The method raw material sources are easy to get, reaction condition gentleness, and reaction conversion ratio is high, and technique ratio is easier to implement, and produces three wastes discharge amount few in production process, and product yield is greatly improved, and belongs to process for cleanly preparing.
Claims (5)
1. the device taking solid base as catalyst salicylate cyclohexyl, comprise cyclohexanol storage tank (1), it is characterized in that: also comprise chemical material pump (2), cyclohexanol head tank (3), gaultherolin head tank (4), reaction kettle of the esterification (5), fractionating 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 cyclohexanol storage tank (1) is connected with cyclohexanol head tank (3) pipeline through chemical material pump (2), and described cyclohexanol head tank (3), gaultherolin head tank (4) are connected with reaction kettle of the esterification (5) pipeline; The hand hole (53) that is provided with reactor agitator (51) and feeds intake for catalyst on described reaction kettle of the esterification (5); Described reaction kettle of the esterification (5) and described fractionating column A(6) pipeline is connected, described fractionating 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 cyclohexanol head tank (3) pipeline by described anticorrosion product pump (10); Described automatic back-cleaning precision filter (9) is also connected with crude reaction pans (11) by pipeline, is provided with recoil nitrogen inlet (111) on described crude reaction pans (11); Described crude reaction pans (11) are connected with washing kettle (12) through pipeline, and described washing kettle (12) is connected with standing head tank (14) through material shifting pump (13) pipeline; Described standing head tank (14) is connected with autoclave rectifying column (15) by pipeline; Described autoclave rectifying column (15) is through fractionating 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 the temporary tank (18) of product by pipeline.
2. the device taking solid base as catalyst salicylate cyclohexyl as claimed in claim 1, it is characterized in that: on described reaction kettle of the esterification (5) madial wall, be 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. the device taking solid base as catalyst salicylate cyclohexyl as claimed in claim 1 or 2, it is characterized in that: described cyclohexanol storage tank (1) is all provided with lagging facility with cyclohexanol head tank (3) outer wall, on the outer wall of the pipeline between pipeline, cyclohexanol head tank (3) and reaction kettle of the esterification (5) between described cyclohexanol storage tank (1) and cyclohexanol head tank (3), is all provided with heat-insulation layer.
4. the device taking solid base as catalyst salicylate cyclohexyl as claimed in claim 3, is characterized in that: in described automatic back-cleaning precision filter (9), be filled with silk screen filter core (91).
5. the device taking solid base as catalyst salicylate cyclohexyl as claimed in claim 4, is characterized in that: described autoclave rectifying column (15) is filled with CY700 filler.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201521052615.5U CN205241572U (en) | 2015-12-17 | 2015-12-17 | Use device of solid base as own ester of synthetic salicylic acid ring of catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201521052615.5U CN205241572U (en) | 2015-12-17 | 2015-12-17 | Use device of solid base as own ester of synthetic salicylic acid ring of catalyst |
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| Publication Number | Publication Date |
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| CN205241572U true CN205241572U (en) | 2016-05-18 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201521052615.5U Active CN205241572U (en) | 2015-12-17 | 2015-12-17 | Use device of solid base as own ester of synthetic salicylic acid ring of catalyst |
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| CN (1) | CN205241572U (en) |
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