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Cinnamic acid, also known as cinnamic acid, β-phenylacrylic acid, has a molecular formula of C 9 H 8 O 2 , a molecular weight of 148.
16, and a structural formula of
1.
Product performance
White monoclinic crystal with slight cinnamon smell; melting point 133℃, boiling point 300℃, relative density (d 4 4 ) 1.
2475; soluble in ether, benzene, acetone, glacial acetic acid , carbon disulfide and oils, soluble in ethanol , methanol and Chloroform is slightly soluble in water; the structure has two isomers, cis and trans, usually trans isomer
.
2.
Production principle
Benzaldehyde is produced by Perkin reaction with acetic anhydride and sodium acetate
.
3.
Process flow
4.
Technical formula (kg/t)
5.
Main equipment
Condensation reaction kettle, storage tank, steam distillation kettle, centrifuge, neutralization kettle
.
6.
Production process
Put 100kg of benzaldehyde, 150kg of acetic anhydride , and 56kg of sodium acetate into a dry reaction kettle, heat up and reflux for 9h, recover acetic acid at normal pressure to an internal temperature of 140°C, and recover acetic anhydride under reduced pressure until the material is viscous
.
After adding 200kg of hot water to dissolve, the unreacted benzaldehyde is recovered by steam distillation, and the internal temperature is controlled at 102℃±2℃ until no oily substance is evaporated
7.
Laboratory preparation method
In the round bottom flask was added 9.
5g freshly steamed benzaldehyde, 25.
9g freshly steamed acetic anhydride and 12.
6g anhydrous potassium carbonate powder, and heated to reflux for 30min
.
Then add 60mL of water, steam distillation to distill the unreacted benzaldehyde, add 60mL of 10% NaOH, so that the sodium salt of cinnamic acid is dissolved in water, and the filtrate is acidified with hydrochloric acid until the Congo red test paper turns blue
8.
Product Standard
9.
Quality inspection
Assay: using acid-base titration method, titration with KOH ethanol standard solution, phenolphthalein as indicator, drip to the solution as pink as the end point
.
In the formula: c-molar concentration of KOH standard solution, mol/L;
V——Volume of KOH standard solution, mL;
G——The mass of the sample, g
.
10.
Product use
It is mainly used for the preparation of esters and synthetic drugs (such as Xinkeding).
The esters are used to prepare lilac-type floral fragrance materials; also used in the production of growth promoters, long-acting fungicides, and fruit and vegetable preservatives
.
11.
Safety measures
(1) The benzaldehyde used in production is low-toxic and is a dangerous product, with an explosion range (lower limit) of 1.
4%; the raw material acetic anhydride is highly toxic, and it is strongly irritating to the eyes, respiratory tract, and mucous membranes
.
The equipment should be airtight, the operator should wear protective equipment, and the workshop should be well ventilated
.
(2) This product is non-toxic.
It is packaged in a plastic bag lined with a woven bag and stored in a cool, ventilated and dry place to prevent sunlight
.
