Process of polymerization and copolymerization redox of vinyl chloride.

04-07-1969 дата публикации
Номер:
OA0000001416A
Принадлежит: Dynamit Nobel Ag
Контакты:
Номер заявки: 51-00-1964900
Дата заявки: 31-12-1964

[1]

AS AFRICAN AND MALAGASY

[2]

INDUSTRIAL PROPERTY

[3]

P. 887

[4]

Yaounde (Cameroon) Patent classifying international: c08 no. 01416

[5]

o.cm w

[6]

31 December 1964 to 18 hr 36 requested Mn to the OA m P. I-.

[7]

(G.P. no. 51,900) called by the business: The Nobel DynamiiAktiengesellschaft, residing in Germany.

[8]

Delivered 4 July 1969, published at Official ballot no. 1 of 1969. Priority: Patent application deposited in Germany in the n° d-d/39 1 c the 42,155 VInC august 1963 on behalf of the applicant.

[9]

Process for polymerization or copolymerization redox chloride of vinyl. [Disclosure: Dr. Robert BUENING and Gerhard BIER.)

[10]

For the polymerization of vinyl chloride

[11]

at temperatures ranging from - 20 °c - 5 °c and,

[12]

machines are known ascorbic acid, of

[13]

heavy metal salts and hydrogen peroxide or

[14]

methyl hydroperoxide. This type of polyméri -

[15]

ina is typically carried out in the presence of

[16]

small amounts of alcohol. Since the speed

[17]

polymerization exceeds 10% per hour and that

[18]

performs substantially a bulk polymerization,

[19]

the removal of the heat of polymerization has

[20]

difficulties, particularly on an industrial scale.

[21]

A further disadvantage is that the exemplary methods

[22]

polymerization rate is not linear primarily

[23]

the beginning of the polymerization.

[24]

It is known further polymerize chloride

[25]

vinyl at low temperatures with acid ascor -

[26]

nanny-goat, heavy metal salts and peroxides such

[27]

that dilauroyl peroxide, peroxide - diben

[28]

zoyle, cumyl hydroperoxide, hydroperoxide

[29]

in the presence of azo cyclohexanone or light

[30]

THE UV. The polymerization rate can then be adjusted

[31]

uV light by the use of UV light - nts

[32]

initially feel additional technical expenditure

[33]

and, further, the UV light acts adversely on the

[34]

resulting polymerizate.

[35]

The present invention shows that these technical defects does - APs

[36]

not appear, upon polymerization or

[37]

copolymerization with the redox systems mentioned, in UIC -

[38]

by reading from the peroxide cyclohexanyl sulfonyl-acetyl in

[39]

the absence of UV light. The rate of polymerization

[40]

is nearly linear at the start of polymerization.

[41]

The yields per hour lie, according to the tempera -

[42]

ation, in the range of 5 to 10 %, favorably for

[43]

mass polymerization. In accordance with the present

[44]

present invention, the polymerization is carried out to still con -

[45]

erasures between - 8 and - 20 °c in the presence

[46]

from about 8 to 20% by weight with respect to chloride

[47]

vinyl a lower alcohol, such as for example

[48]

methanol.

[49]

Example 1. - Was cooled 300 g of chloride

[50]

vinyl to - 16 °c. Adjuvated, stirring, 1.2 grams

[51]

ascorbic acid in 20 ml of methanol, 2 g of peroxide cyclohexanyl sulfonyl-acetyl in 40 ml of methanol and 2 ml of a solution of iron sulfate to 1 % in water. The temperature was maintained at

[52]

- 16 °c using a cooling bath.

[53]

In the following table that yields after specific time intervals.

[54]

Curing time efficiency

[55]

in minutes grams

[56]

15, 5.9

[57]

30, 12.0

[58]

45, 17.9

[59]

60, 24.2

[60]

75, 30.4

[61]

90, 36.5

[62]

Example 2. - It has reproduced the example 1 with the difference that tone has, in addition, used 30 g of vinyl acetate. The yield of the copolymer was 23.5 g after 60 min to.

[63]

Example 3. - It has reproduced the example 1 with the difference that tone has, in addition, used 10 g of ethyl acrylate. The yield of the copolymer was 18.4 g after 45 min.

ABSTRACT

[64]

The invention concerns:

[65]

The process for the polymerization and copolymerization redox of vinyl chloride, at low temperatures, with implementation of ascorbic acid, salts of heavy metals and peroxides in the absence of UV radiation, consisting basically use peroxide cyclohexanyl sulfonyl-acetyl and carrying out the polymerization between about - 8 and

[66]

- 20 °c in the presence of about 8 to 20% by weight (relative to the vinyl chloride) of a lower alcohol.

Company said:

[67]

THE NOBEL AKTIENGESELLSCHAFTDYNAMIT

[68]

Proxy:

[69]

Dr. Robert Pucheu



[70]

Vinyl chloride is polymerized or copolymerized at - 5 DEG to - 20 DEG C., preferably - 8 DEG to - 20 DEG C., in an organic liquid medium in the presence of ascorbic acid, a heavy metal reducing salt and cyclohexanyl-sulphonyl acetyl peroxide. Specified comonomers are vinyl acetate and ethyl acrylate. The organic liquid may be an alcohol, e.g. methanol. Specified heavy metal salts are ferrous salts such as ferrous sulphate. Examples describe the polymerization of (1) vinyl chloride together with (2) vinyl acetate and (3) ethyl acrylate in the presence of methanol, ascorbic acid, ferrous sulphate and cyclohexanylsulphonyl acetylperoxide at - 16 DEG C.



o.cm w

31 December 1964 to 18 hr 36 requested Mn to the OA m P. I-.

(G.P. no. 51,900) by the Company called: the Nobel DynamiiAktiengesellschaft, residing in Germany.

Delivered 4 July 1969, published at Official ballot no. 1 of 1969.

Priority: Patent application deposited in Germany in the n° d-d/39 1 c the 42,155 VInC august 1963 on behalf of the applicant.

Process for polymerization or copolymerization redox vinyl chloride. [Disclosure: Dr. Robert BUENING and Gerhard BIER.)

For the polymerization of vinyl chloride

at temperatures ranging from - 20 °c - 5 °c and,

machines are known ascorbic acid, of

heavy metal salts and hydrogen peroxide or

methyl hydroperoxide. This type of polyméri -

ina is typically carried out in the presence of

small amounts of alcohol. Since the speed

polymerization exceeds 10% per hour and that

performs substantially a bulk polymerization,

the removal of the heat of polymerization has

difficulties, particularly on an industrial scale.

A further disadvantage is that the exemplary methods

polymerization rate is not linear primarily

the beginning of the polymerization.

It is known further polymerize chloride

vinyl at low temperatures with acid ascor -

nanny-goat, heavy metal salts and peroxides such

that dilauroyl peroxide, peroxide - diben

zoyle, cumyl hydroperoxide, hydroperoxide

in the presence of azo cyclohexanone or light

THE UV. The polymerization rate can then be adjusted

uV light by the use of UV light - nts

initially feel additional technical expenditure

and, further, the UV light acts adversely on the

resulting polymerizate.

The present invention shows that these technical defects does - APs

not appear, upon polymerization or

copolymerization with the redox systems mentioned, in UIC -

by reading from the peroxide cyclohexanyl sulfonyl-acetyl in

the absence of UV light. The rate of polymerization

is nearly linear at the start of polymerization.

The yields per hour lie, according to the tempera -

ation, in the range of 5 to 10 %, favorably for

mass polymerization. In accordance with the present

present invention, the polymerization is carried out to still con -

erasures between - 8 and - 20 °c in the presence

from about 8 to 20% by weight with respect to chloride

vinyl a lower alcohol, such as for example

methanol.

Example 1. - Was cooled 300 g of chloride

vinyl to - 16 °c. Adjuvated, stirring, 1.2 grams

ascorbic acid in 20 ml of methanol, 2 g of peroxide cyclohexanyl sulfonyl-acetyl in 40 ml of methanol and 2 ml of a solution of iron sulfate to 1 % in water. The temperature was maintained at

- 16 °c using a cooling bath.

In the following table that yields after specific time intervals.

Curing time efficiency in minutes grams

15, 5.9 30, 12.0

45, 17.9

60, 24.2

75, 30.4 90, 36.5

Example 2. - It has reproduced the example 1 with the difference that tone has, in addition, used 30 g of vinyl acetate. The yield of the copolymer was 23.5 g after 60 min to.

Example 3. - It has reproduced the example 1 with the difference that tone has, in addition, used 10 g of ethyl acrylate. The yield of the copolymer was 18.4 g after 45 min.

ABSTRACT

The invention concerns:

The process for the polymerization and copolymerization redox of vinyl chloride, at low temperatures, with implementation of ascorbic acid, salts of heavy metals and peroxides in the absence of UV radiation, consisting basically use peroxide cyclohexanyl sulfonyl-acetyl and carrying out the polymerization between about - 8 and

- 20 °c in the presence of about 8 to 20% by weight (relative to the vinyl chloride) of a lower alcohol.

Company said:

THE NOBEL AKTIENGESELLSCHAFTDYNAMIT

Proxy:

Dr. Robert Pucheu



CPC - классификация

CC0C08C08FC08F1C08F14C08F14/C08F14/0C08F14/06

IPC - классификация

CC0C08C08FC08F1C08F14C08F14/C08F14/0C08F14/06