CN107903167A

CN107903167A - A kind of low smell zinc stearate preparation method

Info

Publication number: CN107903167A
Application number: CN201711161529.1A
Authority: CN
Inventors: 吴旅良; 洪颖; 熊洪龙
Original assignee: JIANGXI HONGYUAN CHEMICAL CO Ltd
Current assignee: JIANGXI HONGYUAN CHEMICAL CO Ltd
Priority date: 2017-11-21
Filing date: 2017-11-21
Publication date: 2018-04-13

Abstract

A kind of low smell zinc stearate preparation method is that aliphatic acid is put into reaction kettle, opens stirring heating, after its melting, under the conditions of 0.01 0.02 MPa, 90 DEG C, 10 15min are evacuated by micro-vacuum, to remove the low boiling point molecule containing peculiar smell in most of stearic acid；Zinc oxide and catalyst are sequentially added afterwards, is warming up to 130 135 DEG C, opens 0.03 0.04MPa of vacuum, low vacuum is carried out and eliminates the unusual smell operation, and from milky being changed into clear up to reaction solution color, i.e. the reaction was complete；0.05 0.08 MPa of vacuum is opened afterwards, is carried out high vacuum and is eliminated the unusual smell operation, finally discharging crushing.The low smell zinc stearate preparation method of the present invention, due to eliminating the unusual smell technology with three rank vacuum of original creation during the reaction, obtained zinc stearate smell is lower, purity higher is completely suitable for low smell plastic field.

Description

A kind of low smell zinc stearate preparation method

Technical field

The present invention relates to rubber and plastics auxiliaries field, especially a kind of low smell zinc stearate preparation method.

Background technology

The application of plastics on the living conditions is more and more, low VOC, low as people are to ride comfort, healthy and safe requirement The plastics of smell are favored be subject to vast producer, especially upper in the application such as auto plastics, Yoga mat, have gradually formed low smell Plastic industry.Zinc stearate also has the corresponding industry low as common auxiliary agent in plastics-production in low smell plastic field Odor requirements, it is necessary to tested by corresponding smell, generally require smell Deng Ji≤2.Existing smell grading reference, is divided into 1- 6 grades, 1 grade of evaluation criterion：It cannot experience；2 grades of evaluation criterions：It can experience, it is unobstructive；3 grades of evaluation marks It is accurate：Can substantially it experience, but without too big obstruction；4 grades of evaluation criterions：There is obstruction；5 grades of evaluation criterions：There is larger obstruction；6 Level evaluation criterion：It is difficult to endure.

In recent years, production zinc stearate mainly has two methods：One kind is produced using double decomposition, first in stearic acid Caustic soda is added to carry out neutralization reaction, then zincification salt carries out metathesis reaction, and the hard of monomer is formed after dehydration, dry, crushing, packaging Resin acid zinc, the zinc stearate oder levels of output are general >=and 3, and purity is low, is not suitable for low smell plastic field；Second of side Method application colter machine or kneader directly react stearic acid and zinc oxide, catalyst at a certain temperature produces monomer Zinc stearate, the zinc stearate of output is high compared with the first purity, but oder levels are generally >=2, are not also suitable for low smell plastic Field.

The content of the invention

It is an object of the invention to provide a kind of low smell zinc stearate preparation method, the preparation method technique is simple, institute The zinc stearate oder levels of preparation are less than or equal to 2 grades.

A kind of low smell zinc stearate preparation method of the present invention is that aliphatic acid is put into reaction kettle, opens stirring and rises Temperature is to 80-90 DEG C, and after its melting, under the conditions of 0.01-0.02 MPa, 90 DEG C, 10-15min is evacuated by micro-vacuum, with Remove the low boiling point molecule containing peculiar smell in most of stearic acid；Zinc oxide and catalyst, zinc oxide and fat are sequentially added afterwards The mass ratio of fat acid is 15-17:100, catalyst is divided into main effect catalyst and subsidiary catalyst, main effect catalyst for glacial acetic acid or Hydrogen peroxide or monohydric alcohol or polyalcohol or citric acid, subsidiary catalyst are water, and the addition of main effect catalyst is the 2- of aliphatic acid 2.5%, the addition of subsidiary catalyst is 5 times of main effect catalyst, is warming up to 130-135 DEG C, after keeping the temperature 30min, opens vacuum 0.03-0.04MPa, carries out low vacuum and eliminates the unusual smell operation, and being changed into clear from milky up to reaction solution color reacts Completely；Vacuum 0.05-0.08 MPa are opened afterwards, are carried out high vacuum and are eliminated the unusual smell operation, duration 20-25min, finally discharges Crush.

The present invention a kind of low smell zinc stearate preparation method, aliphatic acid selection using palmitic acid, hydrogenated oil and fat, stearic acid as Selection, design parameter is C14≤1%, C16：55-61%, C18：39-44%, acid number：205-211mgKOH/g, iodine number≤0.5 gI2/100g；Zinc oxide：Indirect method manufactures, content >=99.7%, moisture≤0.3%, 325 mesh percent of pass 99.9% of fineness；It is micro- true During sky eliminates the unusual smell, the low boiling point molecule of the peculiar smell contained in most of stearic acid can be removed, low vacuum can avoid stearic acid Molecule scatters and disappears；During low vacuum eliminates the unusual smell, after zinc oxide and catalyst is finished, more than 80% after material reaction 30min Material is reacted, carries out vacuum at this time and eliminates the unusual smell operation most preferably, farthest reduces out influence of the vacuum to reaction, And further odor molecules can be detached；High vacuum eliminates the unusual smell, which can reach the effect except aqueous vapor, and allow water to steam at the same time Gas further takes away more odor molecules, and temperature of charge can faster be reduced.Due to having used original creation during the reaction Three rank vacuum eliminate the unusual smell technology, and obtained zinc stearate smell is lower, and purity higher is completely suitable for low smell plastic field.

Embodiment

A kind of low smell zinc stearate preparation method is that 100Kg aliphatic acid is put into reaction kettle, opens stirring and is warming up to 80-90 DEG C, after its melting, under the conditions of 0.01-0.02 MPa, 90 DEG C, 15min is evacuated by micro-vacuum；Add successively afterwards Enter 16Kg zinc oxide, 2Kg hydrogen peroxide, 10Kg water, be warming up to 130-135 DEG C, after keeping the temperature 30min, open vacuum 0.03- 0.04MPa, carries out low vacuum and eliminates the unusual smell operation, is changed into clear from milky up to reaction solution color, i.e., the reaction was complete； Vacuum 0.05-0.08 MPa are opened afterwards, are carried out high vacuum and are eliminated the unusual smell operation, duration 20-25min, finally discharging crushing.

Claims

A kind of 1. low smell zinc stearate preparation method, it is characterised in that：Aliphatic acid is put into reaction kettle first, opens stirring 80-90 DEG C is warming up to, after its melting, under the conditions of 0.01-0.02 MPa, 90 DEG C, 10-15min is evacuated by micro-vacuum； Zinc oxide and catalyst are sequentially added afterwards, and catalyst is divided into main effect catalyst and subsidiary catalyst, and main effect catalyst is ice vinegar Acid or hydrogen peroxide or monohydric alcohol or polyalcohol or citric acid, subsidiary catalyst are water, are warming up to 130-135 DEG C, keep the temperature 30min Afterwards, vacuum 0.03-0.04MPa is opened, low vacuum is carried out and eliminates the unusual smell operation, be changed into clarifying from milky up to reaction solution color It is transparent that i.e. the reaction was complete；Vacuum 0.05-0.08 MPa are opened afterwards, are carried out high vacuum and are eliminated the unusual smell operation, duration 20- 25min, finally discharging crush.
A kind of 2. low smell zinc stearate preparation method according to claim 1, it is characterised in that：The zinc oxide with The mass ratio of aliphatic acid is 15-17:100.
A kind of 3. low smell zinc stearate preparation method according to claim 1, it is characterised in that：The main effect catalyst Addition be aliphatic acid 2-2.5%, the addition of subsidiary catalyst is 5 times of main effect catalyst.