CN206033621U - Apparatus for producing of silver aldehyde spices - Google Patents
Apparatus for producing of silver aldehyde spices Download PDFInfo
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- CN206033621U CN206033621U CN201620993918.5U CN201620993918U CN206033621U CN 206033621 U CN206033621 U CN 206033621U CN 201620993918 U CN201620993918 U CN 201620993918U CN 206033621 U CN206033621 U CN 206033621U
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Abstract
The utility model discloses an apparatus for producing of silver aldehyde spices relates to the organic synthesis plant field, including acyl group reation kettle A, awl end stirred tank A, cauldron formula distillation column A, acyl group reation kettle B, awl end stirred tank B, cauldron formula distillation column B, hydrogenation reation kettle, cauldron formula distillation column C, car wash gun and cauldron formula rectifying column. The utility model discloses use isobutylbenzene, propionyl chloride as starting material, through synthetic silver -colored aldehyde after acylation reaction and the hydrogenation dechlorination, used raw materials is easy and the product yield is high, and the commercial size metaplasia of being convenient for is produced, the content that passes through this device messenger side reaction meta -position silver aldehyde and consecutive position silver aldehyde simultaneously is below 0.5% to and with 2 in the silver -colored aldehyde finished product the methyl 3 (4 (2 the methyl propyl), benzyl) propyl alcohol content is controlled below 0.5%, makes silver -colored aldehyde product unimodal content reach more than 98.5%, and fragrance is pure soft, accords with the requirement of essence spices blending.
Description
Technical field：
The utility model is related to organic synthesis plant field, and in particular to a kind of process units of silver-colored aldehyde spices.
Background technology：
Silver-colored aldehyde is the one kind in aromatic series lily of the valley class spices, there are no presence report in nature.Silver-colored aldehyde has one kind
Strongly, lucid and lively lily of the valley fragrance, feels with slight orange perfume bottom rhythm and pure and fresh aldehyde are fragrant.Silver-colored hydroformylation scientific name is referred to as 2- methyl -3
(4- (2- methyl-propyls) phenyl) propionic aldehyde, is colourless to weak yellow liquid, CAS 6658-48-6, EINECS 229-695-0,
It is dissolved in ethanol and most of organic solvents, insoluble in G ＆ W, is practically insoluble in propane diols, it is relatively more steady in alkaline solution
It is fixed therefore similar with the usage of other lily of the valley class synthetic perfumes when using, it is adaptable in high-grade daily chemical essence formula, for U.S.
Hold nursing, perfumed soap, the perfuming in laundry care and other household articles, usage amount is 1～15%.
Silver-colored aldehyde has the strong and pure and fresh lily of the valley fragrance of a flower, therefore is widely used in bouquet type composition, fresh and sweet floral perfume
Can use in right amount, the sense fragrant and lasting with profit to strengthen blue or green floweriness head is particularly suitable for for the lily of the valley, cloves, flores aurantii lamp
In numerous bouquet type composition formulas, moreover it is possible to give fresh green grass or young crops perfume fragrance, have preferably with violet ketone and rose class spices
Fragrance harmony.Also can be micro as flavorant, in oranges and tangerines and various Fruity types.
The country does not have the batch production of silver-colored aldehyde at present, and only there is life in the minority enterprise such as international fragrance, Switzerland Qi Huadun in the world
Produce.The dominating process route of silver-colored aldehyde production includes：
One be using isobutyl-benzene in the presence of a large amount of lewis are sour with metering system aldehyde reaction, a step prepares Alpha-Methyl
To isobutyl-benzene propionic aldehyde, the yield of the method only has 10%, while adopting substantial amounts of titanium tetrachloride and BFEE to be complexed
, used as reaction mass, the wastewater flow rate produced after hydrolysis is huge, causes environmental pollution for thing.
Two are reacted under substantial amounts of trifluoracetic acid using isobutylbenzene, butyric anhydride, MAL, are then steamed different
Butylbenzene+butyric acid+trifluoracetic acid mixture, basic hydrolysis obtains silver-colored aldehyde to reactive material in methyl alcohol, and the method is due to a large amount of uses
The very expensive trifluoracetic acid of price and butyric anhydride, production cost are too high.
Three is to carry out chloromethylation, then and methenamine in the presence of formaldehyde, concentrated hydrochloric acid and hydrogen chloride with isobutylbenzene
Carry out Sommelet reactions to obtain to isobutyl-benzene formaldehyde, then with propionic aldehyde alkaline condensation after carry out selective hydrogenation, prepare silver-colored aldehyde,
The method yield only has 20%.
But as the hydrogenation of above-mentioned process can not possibly accomplish absolute selectivity, thus often containing some not by
The impurity such as the undersaturated aldehyde and fraction of 2- methyl -3 (4- (2- methyl-propyls) phenyl) propyl alcohol of reduction, so that affect silver-colored aldehyde
Aroma quality, and product is difficult to purify, and causes fragrance to contain miscellaneous gas.
Utility model content：
Technical problem to be solved in the utility model is that operation is simple, product yield is high, applicable for offer one kind
In industrialized production and can by accessory substance ortho position and meta silver aldehyde and affect aroma quality -3 (4- (2- methyl-propyls) of 2- methyl
Phenyl) silver-colored aldehyde spices of the alcohol content below 0.20% process units.
Technical problem to be solved in the utility model is realized using following technical scheme：
A kind of process units of silver-colored aldehyde spices, including acylation reaction kettle A, cone bottom stirred tank A, still distillation tower A, acyl group
Change reactor B, cone bottom stirred tank B, still distillation tower B, hydrogenation reaction kettle, still distillation tower C, washing kettle and autoclave rectifying column,
Reactant liquor obtained by the acylation reaction kettle A delivers to the stirred tank A extractions of cone bottom by anti-corrosion product pump A, and extraction gained oil reservoir leads to
Cross material shifting pump A deliver to still distillation tower A distillation, distillation kettle liquid proceed to be connected with acylation reaction kettle B to isobutyl-benzene
Acetone head tank, reactant liquor obtained by the acylation reaction kettle B deliver to the stirred tank B extractions of cone bottom, extraction by anti-corrosion product pump B
Gained oil reservoir by material shifting pump B deliver to still distillation tower B distill, distillation kettle liquid proceed to be connected with hydrogenation reaction kettle to different
Butyl-β-chloro- Alpha-Methyl cinnamaldehyde head tank, reactant liquor obtained by the hydrogenation reaction kettle pass through automatic backwash secondary filter
Device filtering catalyst, and filtrate is delivered to into still distillation tower C distillations, distillation kettle liquid delivers to washing kettle washing, washing gained oil reservoir
Autoclave rectifying column rectifying is delivered to by material shifting pump C, silver-colored aldehyde product obtained by rectifying finally delivers to silver-colored aldehyde product temporary storage tank.
Be provided with above the acylation reaction kettle A fed intake by pipeline dichloroethanes head tank, propionyl chloride head tank and
Isobutylbenzene head tank, and acylation reaction kettle A is provided with alchlor and feeds intake hand hole, the cone bottom stirred tank A passes through two chloroethenes
Alkane head tank adds extractant dichloroethanes, is provided with the condenser A and two for reclaiming dichloroethanes above the still distillation tower A
Chloroethanes pans A, is provided with the dimethylformamide head tank and trichlorine fed intake by pipeline above the acylation reaction kettle B
Oxygen phosphorus head tank, the cone bottom stirred tank B passes through dichloroethanes head tank and running water inlet pipeline adds extractant dichloro
Ethane and water, are provided with the condenser B and dichloroethanes pans B for reclaiming dichloroethanes above the still distillation tower B, described to add
The solution of potassium carbonate head tank and ethanol head tank fed intake by pipeline is provided with above hydrogen reactor, and hydrogenation reaction kettle is provided with
Catalyst feeds intake hand hole and the drain with spark arrester, be provided with above the still distillation tower C condenser C that reclaims ethanol and
Ethanol pans, the washing kettle pass through dichloroethanes head tank and running water inlet pipeline add cleaning solvent dichloroethanes and
Water, is provided with distillation spiral-plate heat exchanger and gas-liquid separator above the autoclave rectifying column, first by the dichloroethanes for distilling out
Dichloroethanes vacuum pans are sent into, then the silver-colored aldehyde product for distilling out is sent into into silver-colored aldehyde vacuum pans, silver-colored aldehyde vacuum pans
In silver-colored aldehyde product deliver to silver-colored aldehyde product temporary storage tank eventually through pipeline.
The propionyl chloride head tank and isobutylbenzene head tank control charging time by pump A is added dropwise, to isobutyl-benzene acetone
Head tank and POCl3 head tank control charging time by pump B is added dropwise.
The Alcaine falling film absorbing tower for collecting that reaction generates hydrogen chloride gas, hydrochloric acid is provided with above the acylation reaction kettle A
Film-falling absorption tower is collected the hydrochloric acid for generating is condensed in hydrochloric acid temporary storage tank by graphite condenser.
The running water inlet pipeline for extracting reaction of going out is equipped with the acylation reaction kettle A and acylation reaction kettle B.
The solution of potassium carbonate head tank is prepared kettle by material shifting pump D with potassium carbonate and is connected, and potassium carbonate prepares kettle
It is provided with potassium carbonate to feed intake hand hole and running water inlet pipeline.
The dichloroethanes of recovery is delivered to dichloroethanes head tank by material shifting pump E by the dichloroethanes pans A,
The dichloroethanes of recovery is delivered to dichloroethanes head tank by material shifting pump F by dichloroethanes pans B, and ethanol pans lead to
Cross material shifting pump G and the ethanol of recovery is delivered to into ethanol head tank, dichloroethanes vacuum pans will be returned by material shifting pump H
The dichloroethanes of receipts delivers to dichloroethanes head tank.
Catalyst is recoiled by the automatic back-cleaning precision filter by the ethanol Jing material shifting pump I of ethanol head tank
Wash into hydrogenation reaction kettle.
The beneficial effects of the utility model are：The present invention with isobutylbenzene, propionyl chloride as initiation material, by acylation reaction
With synthesize silver-colored aldehyde after hydrogenation-dechlorination, it is raw materials used to be easy to get and product yield is high, be easy to industrial scale to produce；Simultaneously by this dress
Putting makes the content of side reaction meta silver aldehyde and ortho position silver aldehyde below 0.5%, and by -3 (4- of 2- methyl in silver-colored aldehyde finished product
(2- methyl-propyls) phenyl) alcohol content controls, below 0.5%, to make the unimodal content of silver-colored aldehyde product reach more than 98.5%, and
And aroma of pure is soft, meet the requirement of essence and flavoring agent blending.
Description of the drawings：
Fig. 1 is structural representation of the present utility model；
1- dichloroethanes head tanks；2- propionyl chloride head tanks；3- isobutylbenzene head tanks；4- acylation reaction kettle A；5- is added dropwise
Pump A；6- alchlors feed intake hand hole；7- Alcaine falling film absorbing towers；8- graphite condensers；9- hydrochloric acid temporary storage tanks；10- anti-corrosion materials
Pump A；11- bores bottom stirred tank A；12- material shifting pump A；13- still distillation tower A；14- condenser A；15- dichloroethanes pans
A；16- material shifting pump E；17- dimethylformamide head tanks；18- is to isobutyl-benzene acetone head tank；19- POCl3s are high
Position groove；20- is added dropwise pump B；21- acylation reaction kettle B；22- anti-corrosion product pump B；23- bores bottom stirred tank B；24- material shifting pumps
B；25- still distillation tower B；26- condenser B；27- dichloroethanes pans B；28- material shifting pump F；29- potassium carbonate is prepared
Kettle；30- potassium carbonate feeds intake hand hole；31- material shifting pump D；32- solution of potassium carbonate head tanks；33- is to isobutyl group-β-chloro- α-first
Base cinnamaldehyde head tank；34- ethanol head tanks；35- hydrogenation reaction kettles；36- catalyst feeds intake hand hole；37- drains；38-
Automatic back-cleaning precision filter；39- material shifting pump I；40- still distillation tower C；41- condenser C；42- ethanol pans；
43- material shifting pump G；44- washing kettles；45- material shifting pump C；46- autoclave rectifying columns；47- spiral-plate heat exchangers；48- gas-liquids
Separator；49- dichloroethanes vacuum pans；50- silver aldehyde vacuum pans；51- silver aldehyde product temporary storage tanks；52- materials are shifted
Pump H；53- running water inlet pipelines.
Specific embodiment：
In order that technological means, creation characteristic, reached purpose and effect that the utility model is realized are easy to understand, under
Face combines and is specifically illustrating, and the utility model is expanded on further.
As shown in figure 1, being provided with the dichloroethanes head tank 1, propionyl chloride fed intake by pipeline above acylation reaction kettle A4
Head tank 2 and isobutylbenzene head tank 3, propionyl chloride head tank and isobutylbenzene head tank control charging time by pump A5 is added dropwise, and
Acylation reaction kettle A is provided with alchlor and feeds intake hand hole 6, is provided with collection reaction and generates hydrogen chloride above acylation reaction kettle A
The Alcaine falling film absorbing tower 7 of gas, Alcaine falling film absorbing tower are collected the hydrochloric acid for generating is condensed in hydrochloric acid by graphite condenser 8
In temporary storage tank 9, reactant liquor obtained by acylation reaction kettle A delivers to the stirred tank A11 extractions of cone bottom by anti-corrosion product pump A10, bores bottom
Stirred tank A adds extractant dichloroethanes, extraction gained oil reservoir to send by material shifting pump A12 by dichloroethanes head tank
Distill to still distillation tower A13, above still distillation tower A, be provided with the condenser A14 and dichloroethanes acceptance for reclaiming dichloroethanes
The dichloroethanes of recovery is delivered to dichloroethanes head tank by material shifting pump E16 by tank A15, dichloroethanes pans A, distillation
Kettle liquid proceed to be connected with acylation reaction kettle B21 to isobutyl-benzene acetone head tank 18, be provided with logical above acylation reaction kettle B
Dimethylformamide head tank 17 and POCl3 head tank 19 that piping feeds intake, to isobutyl-benzene acetone head tank and trichlorine
Oxygen phosphorus head tank controls charging time by pump B20 is added dropwise, and reactant liquor obtained by acylation reaction kettle B passes through anti-corrosion product pump B22
The stirred tank B23 extractions of cone bottom are delivered to, cone bottom stirred tank B passes through dichloroethanes head tank and running water inlet pipeline 53 adds extraction
Solvent dichloroethanes and water, extraction gained oil reservoir deliver to still distillation tower B25 distillations, still distillation by material shifting pump B24
The condenser B26 and dichloroethanes pans B27 for reclaiming dichloroethanes is provided with above tower B, and dichloroethanes pans B passes through material
The dichloroethanes of recovery is delivered to dichloroethanes head tank by shifting pump F28, and distillation kettle liquid proceeds to what is be connected with hydrogenation reaction kettle 35
To isobutyl group-β-chloro- Alpha-Methyl cinnamaldehyde head tank 33, the potassium carbonate fed intake by pipeline is provided with above hydrogenation reaction kettle molten
Liquid head tank 32 and ethanol head tank 34, solution of potassium carbonate head tank are prepared kettle 29 by material shifting pump D31 with potassium carbonate and are connected
Connect, potassium carbonate is prepared kettle and is provided with potassium carbonate and feeds intake hand hole 30 and running water inlet pipeline, and hydrogenation reaction kettle is provided with catalysis
Agent feeds intake hand hole 36 and the drain with spark arrester 37, and reactant liquor obtained by hydrogenation reaction kettle passes through automatic backwash secondary filter
38 filtering catalyst of device, and backwashed catalyst into hydrogenation reaction by the ethanol Jing material shifting pump I39 of ethanol head tank
Kettle, gained filtrate deliver to still distillation tower C40 distillations, are provided with the condenser C41 and ethanol for reclaiming ethanol above still distillation tower C
The ethanol of recovery is delivered to ethanol head tank by material shifting pump G43 by pans 42, ethanol pans, and distillation kettle liquid is delivered to and washed
Wash kettle 44 to wash, washing kettle passes through dichloroethanes head tank and running water inlet pipeline adds cleaning solvent dichloroethanes and water,
Washing gained oil reservoir delivers to 46 rectifying of autoclave rectifying column by material shifting pump C45, is provided with distillation spiral shell above autoclave rectifying column
The dichloroethanes for distilling out first is sent into dichloroethanes vacuum pans 49, dichloro by spiral plate exchanger 47 and gas-liquid separator 48
The dichloroethanes of recovery is delivered to dichloroethanes head tank by material shifting pump H52 by ethane vacuum pans, then will be distilled out
Silver-colored aldehyde product send into silver-colored aldehyde vacuum pans 50, the silver-colored aldehyde product in silver-colored aldehyde vacuum pans delivers to silver-colored aldehyde eventually through pipeline
Product temporary storage tank 51.The running water inlet pipeline 53 for extracting reaction of going out is equipped with acylation reaction kettle A and acylation reaction kettle B.
General principle of the present utility model and principal character and advantage of the present utility model has been shown and described above.One's own profession
The technical staff of industry it should be appreciated that the utility model is not restricted to the described embodiments, described in above-described embodiment and specification
Simply illustrate principle of the present utility model, on the premise of without departing from the utility model spirit and scope, the utility model is also
Various changes and modifications are had, these changes and improvements are both fallen within the range of claimed the utility model.The utility model
Claimed scope is by appending claims and its equivalent thereof.
Claims (8)
1. a kind of process units of silver-colored aldehyde spices, it is characterised in that：Steam including acylation reaction kettle A, cone bottom stirred tank A, autoclave
Evaporate tower A, acylation reaction kettle B, cone bottom stirred tank B, still distillation tower B, hydrogenation reaction kettle, still distillation tower C, washing kettle and kettle
Formula rectifying column, reactant liquor obtained by the acylation reaction kettle A deliver to the stirred tank A extractions of cone bottom by anti-corrosion product pump A, extract institute
Obtain oil reservoir and still distillation tower A distillations are delivered to by material shifting pump A, distillation kettle liquid proceeds to right with what acylation reaction kettle B was connected
Isobutyl-benzene acetone head tank, reactant liquor obtained by the acylation reaction kettle B deliver to cone bottom stirred tank B by anti-corrosion product pump B
Extraction, extraction gained oil reservoir deliver to still distillation tower B distillations by material shifting pump B, and distillation kettle liquid is proceeded to and hydrogenation reaction kettle
It is connected to isobutyl group-β-chloro- Alpha-Methyl cinnamaldehyde head tank, reactant liquor obtained by the hydrogenation reaction kettle passes through automatic backflushing
Accurate filter filtering catalyst is washed, and filtrate is delivered to into still distillation tower C distillations, distillation kettle liquid is delivered to washing kettle washing, washed
Wash gained oil reservoir and autoclave rectifying column rectifying is delivered to by material shifting pump C, silver-colored aldehyde product obtained by rectifying finally delivers to silver-colored aldehyde product
Temporary storage tank.
2. the process units of silver-colored aldehyde spices according to claim 1, it is characterised in that：Above the acylation reaction kettle A
Dichloroethanes head tank, propionyl chloride head tank and the isobutylbenzene head tank fed intake by pipeline is provided with, and on acylation reaction kettle A
It is provided with alchlor to feed intake hand hole, the cone bottom stirred tank A adds extractant dichloroethanes, institute by dichloroethanes head tank
State and above still distillation tower A, be provided with the condenser A and dichloroethanes pans A for reclaiming dichloroethanes, the acylation reaction kettle B
Top is provided with the dimethylformamide head tank and POCl3 head tank fed intake by pipeline, and the cone bottom stirred tank B passes through
Dichloroethanes head tank and running water inlet pipeline add extractant dichloroethanes and water, set above the still distillation tower B
There is the condenser B and dichloroethanes pans B for reclaiming dichloroethanes, above the hydrogenation reaction kettle, be provided with what is fed intake by pipeline
Solution of potassium carbonate head tank and ethanol head tank, and hydrogenation reaction kettle is provided with catalyst and feeds intake hand hole and putting with spark arrester
Eat dishes without rice or wine, above the still distillation tower C, be provided with the condenser C and ethanol pans for reclaiming ethanol, the washing kettle passes through dichloro
Ethane head tank and running water inlet pipeline add cleaning solvent dichloroethanes and water, are provided with distillation above the autoclave rectifying column
With spiral-plate heat exchanger and gas-liquid separator, the dichloroethanes for distilling out is sent into into dichloroethanes vacuum pans first, then will be steamed
The silver-colored aldehyde product for distillating sends into silver-colored aldehyde vacuum pans, and the silver-colored aldehyde product in silver-colored aldehyde vacuum pans delivers to silver eventually through pipeline
Aldehyde product temporary storage tank.
3. the process units of silver-colored aldehyde spices according to claim 2, it is characterised in that：The propionyl chloride head tank and isobutyl
Benzene head tank controls charging time by pump A is added dropwise, to isobutyl-benzene acetone head tank and POCl3 head tank by being added dropwise
Pump B controls charging time.
4. the process units of silver-colored aldehyde spices according to claim 1, it is characterised in that：Above the acylation reaction kettle A
The Alcaine falling film absorbing tower for collecting that reaction generates hydrogen chloride gas is provided with, Alcaine falling film absorbing tower will be condensed by graphite condenser
The hydrochloric acid of generation is collected in hydrochloric acid temporary storage tank.
5. the process units of silver-colored aldehyde spices according to claim 1, it is characterised in that：The acylation reaction kettle A and acyl
The running water inlet pipeline for extracting reaction of going out is equipped with glycosylation reaction kettle B.
6. the process units of silver-colored aldehyde spices according to claim 2, it is characterised in that：The solution of potassium carbonate head tank leads to
Cross material shifting pump D and potassium carbonate and prepare kettle and be connected, and potassium carbonate preparation kettle is provided with that potassium carbonate feeds intake hand hole and running water enters
Mouth pipeline.
7. the process units of silver-colored aldehyde spices according to claim 2, it is characterised in that：The dichloroethanes pans A leads to
Cross material shifting pump E and the dichloroethanes of recovery is delivered to into dichloroethanes head tank, dichloroethanes pans B passes through material shifting pump
The dichloroethanes of recovery is delivered to dichloroethanes head tank by F, and the ethanol of recovery is delivered to by ethanol pans by material shifting pump G
Ethanol head tank, it is high-order that the dichloroethanes of recovery is delivered to dichloroethanes by material shifting pump H by dichloroethanes vacuum pans
Groove.
8. the process units of silver-colored aldehyde spices according to claim 1, it is characterised in that：The automatic backwash secondary filter
Device is backwashed catalyst into hydrogenation reaction kettle by the ethanol Jing material shifting pump I of ethanol head tank.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201620993918.5U CN206033621U (en) | 2016-08-30 | 2016-08-30 | Apparatus for producing of silver aldehyde spices |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620993918.5U CN206033621U (en) | 2016-08-30 | 2016-08-30 | Apparatus for producing of silver aldehyde spices |
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| CN206033621U true CN206033621U (en) | 2017-03-22 |
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