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13/2/2014 CN103012132A Patent - Preparazione di acetato prenil - Google Patents
https://www.google.com/patents/CN103012132A?cl=en&dq=%221191-16-8%22+OR+%22prenyl+acetate%22+OR+%223-methyl-2-butenyl+acetate%22+… 1/3
Brevetti
CN103012132 A
Tipo di pubblicazione Applicazione
Numero della domanda CN 201210570822
Data di pubblicazione Apr 3, 2013
Data di deposito 26 dicembre 2012
Data di priorità 26 dicembre 2012
Inventori
Richiedente
Esporta citazione BiBTeX , EndNote , RefMan
Classificazione (2), Eventi legali (2)
Collegamenti esterni: SIPO , Espacenet
CLAIMS (3) tradotte dal cinese
1 sorbitol ester, characterized by comprising the steps of: (1) into the reactor in
acetic anhydride and sodium acetate, heated to 100 ° C after the dropwise
addition, glutaric enol 100-110 ° c, After dropping the reaction temperature at this
temperature for 2 hours; (2) After completing the reaction of step (I) the amount of
water was added, stirring, standing, falling layer of water, to obtain a crude liquid
sorbitol esters; the crude liquid esters of sorbitol was added anhydrous sodium
carbonate adjusted to PH 7; (3) of the crude liquid sorbitol ester distillation,
collecting 70-80 ° C / 50mmHg fractions, sorbitol esters have finished.
(2) as claimed in claim 1, wherein a sorbitol ester, characterized in that:
acetic anhydride: glutaric enol: mol of sodium acetate and I: 1. 7-1. 9: 0.
05.
3 as claimed in claim 1, wherein a sorbitol ester, characterized in that:
in step (2), wherein the amount of water added, the amount of water in
step (I) 10% of the weight of the material.
Metodo di preparazione di acetato prenilCN 103012132 A
ASTRATTO
L'invenzione descrive un metodo di preparazione di acetato prenil , che
comprende le seguenti fasi: (1) l'aggiunta di anidride acetica e acetato di sodio in
un recipiente di reazione, riscaldamento a 100 gradi C, aggiungendo dropwisely
pentadienol a 100-110 gradi C, quindi eseguire temperatura costante reazione per
2 ore alla temperatura; (2) Dopo la reazione, aggiungendo una quantità adeguata
di acqua nella soluzione della fase (1), mescolando, in piedi, separano per
rimuovere l'acqua al livello inferiore in modo da ottenere grezzo acetato prenil
liquido ; aggiungendo carbonato di sodio anidro in greggio acetato prenil liquido
per regolare il pH a 7; (3) rettificare il greggio acetato prenil liquido, raccogliendo
una frazione del 70-80 DEG C/50 mmHg avere la acetato prenil prodotto finito. L'invenzione è semplice nella preparazione condizioni di reazione, molto elevati in resa
del prodotto, e particolarmente adatto per la produzione industriale; l' acetato prenil resa del prodotto è superiore al 88%, e il contenuto dopo rettifica è fino a più di
97%.
DESCRIZIONE tradotto dal cinese
Sorbitol esters thereof
Technology
[0001] The present invention relates to the field of chemical technology, in
particular to a method for preparing esters of sorbitol.
BACKGROUND
[0002] sorbitol esters (isopentenyl acetate ester China; - prenyl acetate; acid -2 -
isopentenyl esters; 3,3 -
Acetic acid allyl ester; 3_-2 - butenyl acetate; 3,3 - dimethyl allyl acetate;
Titanium -3 - methyl - 2 - butenyl acetate; acid 3 - methyl-2 - butenyl ester; 3 -
methyl - 2 - butene-1 - acetate) was prepared. Sorbitol esters existing system by
a method for producing prenyl chloride and sodium acetate as raw interaction
system. As the solid sodium acetate, the reaction to the introduction of toluene
as a solvent, not only reduces the production capacity, and the subsequent
process will increase the problem of solvent recovery. Meanwhile chlorinated
isoprene there is damage to the environment, the human body after inhalation
obvious damage lung tissue, and the price is higher. The reaction of a large amount of salt water burden on the environment.
SUMMARY OF THE INVENTION
[0003] The object of the present invention is to provide a method for preparing esters of sorbitol, this production method is
simple
Single reaction without solvent, improve equipment utilization, product yield. Raw materials for environmental damage is
small, the reaction does not produce wastewater harm to the environment.
[0004] The present invention through the following technical solution:
One kinds of sorbitol ester, comprising the steps of:
(1) into the reactor in acetic anhydride and sodium acetate, heated to 100 ° C after the dropwise addition, glutaric 100-110 ° c
alcohol was added dropwise at this temperature for 2 hours under constant;
(2) After completing the reaction of step (I) the amount of water was added, stirring, standing, falling layer of water, to obtain a
crude liquid sorbitol esters; sorbitol ester To the crude liquid was added to adjust the PH of anhydrous sodium carbonate to
7;
(3) the crude liquid sorbitol ester distillation, collecting 70-80 ° C / 50mmHg fractions, sorbitol esters have finished.
[0005] The acetic anhydride: glutaric alcohol: 1:1 molar sodium acetate. 7-1 9: 0.05.
[0006] Step (2) The amount of water added, the amount of water in step (I) to 10% by weight of the material.
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Numero dipubblicazione
CineseInglese
"1191-16-8" OR "prenyl acetate" OR "3-methyl-2-butenyl acetate" OR "3-methyl-2-buten-1-yl acetate"gian.colla @ aliceposta.it
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13/2/2014 CN103012132A Patent - Preparazione di acetato prenil - Google Patents
https://www.google.com/patents/CN103012132A?cl=en&dq=%221191-16-8%22+OR+%22prenyl+acetate%22+OR+%223-methyl-2-butenyl+acetate%22+… 2/3
[0007] The present invention compared with the prior art has the following advantages:
The preparation is simple reaction conditions, product yield is high, especially for the industrial production of the present
invention can be widely used in daily chemical flavor formulations.
[0008] sorbitol ester product yield of 88% and above, after distillation content of up to 97% and above.
[0009] Description of Embodiments Example 1
The molar ratio of acetic anhydride: glutaric enol: Sodium acetate = 1: 1.8: 0.05.
[0010] I) to ensure that the reactor clean and dry. The 1020 kg of acetic anhydride with a pump into the reactor and adding 41
kg of sodium acetate was heated to 100 ° c after the dropwise addition, glutaric enol 100-110 ° c 1548 kg, about 4 hours After
completion of dropping, in thermostatic temperature for 2 hours; reaction end: Shu dienol feed solution containing less than
O. 5%.
[0011] reaction equation:
2) After the reaction, the crude product was added to 260 kg of water, stirred, allowed to stand. Fall layer of water, to obtain a
crude liquid sorbitol esters of 2420 kg. To the crude liquid sorbitol esters of anhydrous sodium carbonate was added to adjust
the Ph 7.
[0012] 3) the step (2) Ph adjusted to 7 after the crude liquid sorbitol ester distillation, collecting 70-80 ° C / 50mmHg for
distillate product sorbitol esters, sorbitol esters to obtain 2136 kg product, the GC analysis, finished pear ester content of
97.1%, sorbitol ester product yield was 88.3%.
[0013] Example 2
The molar ratio of acetic anhydride: glutaric enol: Sodium acetate = 1: 1.9: 0.05.
[0014] I) to ensure that the reactor clean and dry. The 1020 kg of acetic anhydride with a pump into the reactor and adding 41
kg of sodium acetate was heated to 100 ° c after the dropwise addition, glutaric enol 100-110 ° c 1634 kg, about 4 hours After
completion of dropping, in thermostatic temperature for 2 hours; reaction end: Shu dienol feed solution containing less than
O. 5%.
[0015] reaction equation:
2) After the reaction, the crude product was added to 280 kg of water, stirred, allowed to stand. Fall layer of water, to obtain a
crude liquid sorbitol esters of 2430 kg. To the crude liquid sorbitol esters of anhydrous sodium carbonate was added to adjust
the Ph 7.
[0016] 3) step 2) Ph adjusted to 7 after the crude liquid sorbitol ester distillation, collecting 70-80 ° C / 50mmHg for distillate
product sorbitol esters, sorbitol esters to obtain 2128 kg product by GC analysis, finished pear ester content of 97.2%,
sorbitol ester product yield was 87.6%.
[0017] Example 3
The molar ratio of acetic anhydride: glutaric enol: Sodium acetate = 1: 1.7: 0.05.
[0018] I) to ensure that the reactor clean and dry. The 1020 kg of acetic anhydride with a pump into the reactor and adding 41
kg of sodium acetate was heated to 100 ° c after the dropwise addition, glutaric enol 100-110 ° c 1462 kg, about 4 hours After
completion of dropping, in thermostatic temperature for 2 hours; reaction end: Shu dienol feed solution containing less than
O. 5%.
[0019] reaction equation:
2) After the reaction, the crude product was added to 260 kg of water, stirred, allowed to stand. Fall layer of water, to obtain a
crude liquid sorbitol esters of 2180 kg. To the crude liquid sorbitol esters of anhydrous sodium carbonate was added to adjust
the Ph 7.
[0020] 3) the step (2) Ph adjusted to 7 after the crude liquid sorbitol ester distillation, collecting 70-80 ° C / 50mmHg for
distillate product sorbitol esters, sorbitol esters to obtain 1912 kg product, the GC analysis, finished pear ester content of
97.3%, sorbitol ester product yield was 87.7%.
13/2/2014 CN103012132A Patent - Preparazione di acetato prenil - Google Patents
https://www.google.com/patents/CN103012132A?cl=en&dq=%221191-16-8%22+OR+%22prenyl+acetate%22+OR+%223-methyl-2-butenyl+acetate%22+… 3/3
CLASSIFICAZIONE
Classificazione internazionale C07C67/08 , C07C69/145
EVENTI LEGALI
Data Codice Evento Descrizione
1 Maggio 2013 C10 Richiesta di esame nel merito
Apr 3, 2013 C06 Pubblicazione
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