FI68412C - FOERFARANDE FOER FRAMSTAELLNING AV EN HUVUDSAKLIGEN STABIL VATTENDISPERSION AV KOLOFONIUMMATERIAL I NAERVARO AV ETT KATIONISKT EMULGERMEDEL - Google Patents

Description

NOTICE 6841 2

patent application Offenlegungsschrift

C (45) Patent ayär.ne-tty 10 09 1985 Patent aeddolat. C 08 L 93/0 **, C 08 J 3/02, 1 (51) Kv.lk.4 / lnt.CI. B 01 F 17/18 // D 21 H 3/3 * »FINLAND - FINLAND (21) Patent application - Patentansökning 771928 (22) Application date - Ansöknlngsdag 20 06 77 iFh '' (23) Starting date - Giltighetsdag 20.06.77 (41) Has become public - Blivit offentlig 22 01 78

National Board of Patents and Registration Date of display and publication

Patent- och registerstyrelsen 1 'Ansökan utlagd och utl.skriften publicerad 31 · 05.85 (32) (33) (31) Privilege claimed - Begärd priority 21 .07.76 Sweden-Sweden (SE) 7808289-0 (71) KemaNobel AB, Box 11005 , S-100 61 Stockholm 11, Sweden-Sweden (SE) (72) Claes Olof Axel Lundin, Saltsjö-Boo, Sweden-Sweden (SE) (7 * 0 Oy Jalo Ant-Wuorinen Ab (5 ^) Method for rosin Laine mainly The present invention relates to a process for the preparation of homologous dispersible and aqueous dispersions of rosin substances according to the invention. acid.

Rosin dispersions are used in the paper industry for pulp and surface sizing of cellulose and various methods for preparing dispersions are known. U.S. Patent 3,565,755 describes rosin dispersions prepared by a solvent process. According to Swedish patent applications 7406984-0 and 7410018-1, aqueous dispersions of rosin without solvent are prepared by homogenization at high pressure and high temperature. According to both applications, anionic stabilizers such as rosin soap, alkylbenzenesulfonic acid salts, etc. are used to prepare stable dispersions by using anionic stabilizers after avoiding reactions with rosin acids in the rosin.

According to the invention, it has been found that mainly stable rosin dispersions can be prepared by using certain cationic nitrogen-containing emulsifiers which give the resin particles a positive surface charge.

Since cellulose fibers have a negative surface charge, it is preferable to use positively charged resin particles to achieve good retention. Cationic compounds generally react with rosin acids in an ion exchange reaction with hydrogen ions, whereby the cationic group is lost.

According to the invention, it has been found that by using certain types of cationic nitrogen-containing compounds, it is possible to prepare mainly stable rosin dispersions despite this reaction, so as to obtain a cationic dispersion with improved retention in negatively charged cellulose.

The present invention thus relates to a process for the preparation of substantially stable dispersions of rosin, in which a preheated mixture of rosin material and water is homogenized at a temperature of 150-190 ° C. The invention is characterized in that the homogenization is carried out using a cationic nitrogen-containing emulsifier consisting of quaternary monoammonium compounds having at least one higher aliphatic group having 10 to 22 carbon atoms and a) quaternary di- or polyammonium compounds containing at least one higher -22 carbon atom aliphatic groups, b) combinations of fully or partially neutralized homo- or copolymers of vinylpyridine, or c) fully or partially neutralized homo- or copolymers of ethyleneimine.

By rosin substance is meant known types of rosin, such as carrier, wood and tall oil rosin. The rosin material may be crude or refined, proprotionated, hydrogenated, modified and / or fortified in a known manner. Preferably, iodine- or formaldehyde-treated tall oil rosin is used to avoid crystallization. The rosin may be fortified, i.e. it may have reacted with an α, β-unsaturated polybasic acid or its anhydride, e.g. fumaric acid, maleic acid, itaconic acid and their 6841 2 3 anhydrides.

The quaternary mono-, di- and polyammonium compounds contain at least one higher aliphatic group having from 10 to 22 carbon atoms. The aliphatic group may be substituted and contain amide, ether or ester groups. The higher aliphatic group is preferably an alkyl group having 12 to 20 carbon atoms.

Particularly good results have been obtained with combinations of quaternary monoammonium compounds and polymers, as well as with combinations of quaternary mono- and diammonium compounds. In these combinations, the weight ratio between the quaternary monoammonium compound and the polymer or quaternary diammonium compound is suitably 1:10 to 10: 1, in particular 1: 0.5 to 1: 3. Combinations of quaternary mono- and diammonium compounds have obtained the best results with monoammonium compounds containing two higher aliphatic groups and diammonium compounds containing one higher aliphatic group.

According to the present method, a preheated mixture of rosin and water is homogenized at a high temperature. The temperature is 150-190 ° C and is chosen to obtain a suitable viscosity and to avoid thermal decomposition of the rosin. The homogenization is preferably carried out in a suitable apparatus at a pressure of about 70 to about 560 kp / cm 2 and the resulting dispersion is cooled.

The present method can be used to prepare dispersions with a high dry matter content, up to 50-60%. The emulsifier is used in an amount of 0.5 to 8% by weight, based on the rosin substance, suitably 1 to 3% by weight.

Dispersions prepared according to the invention are used in a known manner for surface and mass gluing. In pulp sizing, dispersions can be used in conjunction with known paper additive chemicals such as retention aids, alum, etc.

Because the dispersions of the invention are positively charged, significantly less alum is required in bulk sizing compared to sizing with anionic dispersions. Although smaller amounts of alum are used, the retention of fibers and potential fillers remains good. Bulk sizing with dispersions can take place over a wide pH range, from about 4 to about 7.

The invention is explained in more detail in the following embodiments. Parts and percentages refer to parts by weight, respectively, unless otherwise stated.

6841 2 4

Example 1 a) -b);

Dispersions were prepared on a laboratory scale starting from 20 parts by weight of a fortified and formaldehyde-modified pine resin having an acid number of 194, from 1 part by weight of various emulsifiers and from water to 100 parts by weight. The cationic activity of the different dispersions, measured as mobility, was measured by particle high electrophoresis.

Emulsifier Cationic activity at pH 3.5 (u »cm) (V.asa) Combination of N-octadecyl-N-dimethyl, N'-trimethylpropylene diammonium dichloride and dioctadecyldimethylammonium chloride + 5.0 b) dioctadecyldimethylammonium chloride a combination of a partially neutralized vinyl-pyridine copolymer with a nitrogen content of 6.6% in a ratio of 1: 0.26 + 4.5

Example 2: 20 parts by weight of a fortified and formaldehyde-modified pine resin having an acid number of 220 were mixed with 0.92 parts by weight of dimethyldistearylammonium chloride, 0.625 parts by weight of N-octadecyldimethyl-N'-trimethylpropylenediammonium chloride and 100 parts by weight of water. parts. The mixture was heated to 173 ° C and homogenized at 200-220 kp / cm 2. The resulting dispersion was rapidly cooled to 25 ° C. Dry matter content 21.5%. A portion of the dispersion was diluted to a dry matter content of 5%. There was no precipitation in this diluted dispersion after 4 weeks at room temperature.

Example 3: The dispersion according to Example 2 was used to glue the pulp.

On a laboratory sheet machine, sheets were made from bleached sulphate pulp, birch: pine 50/50, ground to 30 ° SR. The pulp concentration was 2% and its pH was about 4.5. 0.3% dry resin dispersion based on dry fibers and 2% alum were added to the pulp. The sheets were compressed, dried for 90 minutes at 65 ° C and conditioned for more than 4 hours at 23 ° C in 50% RH. The sizing effect was determined according to SCAN P 12:64. Result

Claims (3)

5 CobbgQ g / m2 = 26/2. 68412 Example 4; In a manner similar to Example 3, sheets were prepared using a 0/5% dry resin dispersion according to Example 2 at pH 6/5. The pH of the pulp was adjusted by adjusting the pH to about 9 with sodium hydroxide, and after 12 hours, alum, sulfuric acid to pH 6.5, and the resin dispersion were added, respectively. In this case, the Cobb number was 25.7. A process for preparing a substantially stable aqueous dispersion of a rosin by homogenizing a preheated mixture of water and rosin at 150-190 ° C, characterized in that the homogenization is carried out using a cationic nitrogen-containing emulsifier consisting of quaternary aliphatic at least one higher alpha-containing 10-22 carbon atoms. a) quaternary di- or polyammonium compounds containing at least one higher aliphatic group of 10 to 22 carbon atoms, b) fully or partially neutralized homo- or copolymers of vinylpyridine, or c) fully or partially neutralized homo- or partially neutralized homo- or copolymers of ethyleneimine. combinations of copolymers. Process according to Claim 1, characterized in that the quaternary ammonium compounds contain at least one alkyl group having 12 to 20 carbon atoms. Process according to Claim 1 or 2, characterized in that the emulsifier consists of a combination of a quaternary monoammonium compound and a quaternary diammonium compound or a combination of a quaternary monoammonium compound and a wholly or partially neutralized homopolymer or copolymer of vinylpyridine.