HU201367B - Method for producing hydrophilic resin solutions stable in wide range - Google Patents

Abstract

Pine resin and tall resin are used to form esters in a medium of glycols with higher boiling points. The prod. is poured in an atmos. of inert gas, heated, then cooled. The system is saponified using caustic and stablisised by the addition of diamide. The final prod. concn. is achieved by the addition of water.

Description

The present invention relates to a novel process for the preparation of a stable hydrophilic resin emulsion by partial alkaline saponification of resins (preferably pine or tall resins). The resulting product would be glued. respectively. can be used as an additive for dispersion adhesives.

It is known in the paper industry to use a large amount of different pine resin based adhesives. Abietic acid or pine resin in pine resins. its isomers are partially or completely saponified, and the resulting sodium resinate is treated with casein, starch, skin-like protective colloids to increase the stability of the disperse system (see Paper Handbook, Technical Publisher, Budapest, 1980).

The major disadvantage of colloidal systems known in the art as adhesives (e.g., Passageways, Bewoids, or Lacresin glues - see the Paper Industry Manual cited above) is that they remain in a concentration of only 10-20% (solvents mostly; aromatic solvents). stable. At higher concentration ranges (e.g., above 30-35% by weight) the pastes can no longer be stored for longer periods, the phases are separated, and they are sensitive to cold. Liquid resins can be diluted with water at very narrow limits without loss of stability (see Lajos Kovács, Aqueous Polymer Suspensions, Technical Publisher Budapest, 1986).

It is also known. that the properties of saponified resins can be improved with protective colloids. In fact, it is. the resin is approaching 50% by weight and the composition is dense. pasty. it becomes cold after a short stance and becomes unstable.

It is therefore an object of the present invention to provide a process for overcoming the above drawbacks and providing a highly stable, well-manageable papermaking aid that can be diluted over a wide range of concentrations.

The present invention is based on the recognition that the prior art saponification of the resins used as starting materials must be carried out in the presence of certain types of divalent alcohols. As a result, ester derivatives are formed in the system which act as a local emulsifier and keep both the oil / water and water / oil type systems stable.

Surprisingly, it has also been found in our experiments that the stability of the above system can be further enhanced by the addition of urea (presumably by inclusion complexes).

Our discovery also results in significant technological advances, since our method can be used to prepare the hydrophobizing (sizing) material of papermaking fibers together with an additive that increases adhesion of the adhesive in a single reactor with a single chemical step.

Accordingly, the present invention provides a process for preparing a stable hydrophilic resin emulsion by partially alkalinizing saponification of resin species such that rosin resin having a melting point below 100 ° C or rosin resin containing up to 20% by weight of resin is based on the weight of resin. 20-50% by weight

It is mixed with C 4 -C 8 alkylene diol in a molten state at a temperature of 70-95 ° C, preferably in a stream of nitrogen, and 30-50% by weight of the alkali metal hydroxide 25-35% by weight of the resin. solution, ·>

15-25% by weight of urea is then added, followed by the preparation of an aqueous emulsion of 30-70% by weight of the resulting mixture at 50-60 ° C with water, preferably softened water.

In a preferred embodiment of the invention, the alkylene diol is 2-methylpentane-2,4-diol.

The starting material used is pine resin or pine resin containing up to 20% by weight of tall resin. For a more efficient and faster reaction run, the resin is preferably pulverized, preferably in the form of lumps or spheres having a diameter of 2 to 20 mm.

The resin or starting material used as starting material. the melting point of the resin mixture should not exceed 100 ° C, preferably 85-95 ° C.

Sodium potassium hydroxide can be used as the alkali metal hydroxide in the process according to the invention, preferably in an aqueous solution of 25-35% by weight.

For the preparation of aqueous emulsions, it is advisable to use softened water, the hardness of which should not exceed 6-8 German degrees. The aqueous dilution is carried out at a temperature between 50 ° C and 60 ° C to form a very stable emulsion.

The advantages and the advanced nature of the process of the invention are summarized below:

1. The process can be performed in a single reactor using simple technology.

2. The process can be magnified perfectly and, if desired, carried out in increments of hundreds of kg.

3. The product obtained by the process outperforms the known formulations by several parameters.

To prove this, we present the results of comparative experiments:

In the comparison, the following formulations were tested:

Indication Product name Origin of preparation place THE FF-400 The product of Example 1 of the present invention B Furin-3-N Austria C Soreze-500 Turkey

The study included a comparison of sizing properties. In detail:

I. Fiber materials used:

% Soviet Unbleached Sulphite Pulp Cellulose 20% Dunaújváros Bleached Straw Cellulose pH 7.4

II. Envvezőanvagok:

ABC

Solids content (%) 36.7 91.6 91.0 pH 9.7 9.7 11.0

The gluing was done from 3% solution.

The size of the adhesive is 0.5 t% 0.2 t% 0.2 t% (relative to absolute dry fiber).

III. How to publish:

The fibers were soaked for 2 hours and then disintegrated in a disintegrator for 25 minutes. We weighed 6 pieces of 70 g / m sheet into the blender and glued to the amount of glue

HU 201367 fuel was added. After stirring for about 2 minutes, the aluminum sulfate was added, stirred for 2 minutes, and the pH and Al ⁺⁺⁺ concentration were measured.

A sheet was formed which was dried at 90-100 ° C.

ARC. Summary of results:

When comparing the essential properties of the 3 adhesives on the basis of the tests, the following conclusion can be made:

\ LEADER- MATERIALS JELLEMZÓKX. THE B C Ideal pH 4.4-4.6 (between) 4.5 4.4 and 4.8

Surface suction capacity (Cobbfio g / m ^{I. 2} ) 19-20 28 28

V. Evaluation

- with the same amount of fiber and adhesive, the best adhesive was achieved with resin A (19-20 g / m ² ),

- the gluing efficiency of formulations B and C is much less favorable,

- only the two given pH-η functions properly.

The process of the present invention is illustrated by the following examples:

Example I

100 g of powdered pine resin, 2-20 mm in diameter, with 24.9 g (0.21 mol) of 2-methylpentane-2,4-diol with stirrer. melting at 70-95 ° C in a round-bottomed reflux condenser by bubbling nitrogen into the atmosphere. To the homogeneous melt was added 38.9 g (0.45 mol) of a 30% w / w sodium hydroxide solution over 15 minutes with further stirring. After maintaining the upper temperature at 75 ° C, after 15 minutes of the reaction, 21.5 g (0.33 mol) of urea are added to the reaction mixture. The mixture was then cooled to 60 ° C with stirring and mixed with 120 g (ml) of soft water.

Product: 175 g translucent, yellow, 50% emulsion.

Example 2

All were carried out in the same manner as in Example 1 except that 80 g of pine resin and 20 g of tall resin were used as starting materials.

Product: 170 yellow-brown translucent, stable 50% emulsion.

Example 3

All proceed as in Example 1 with the exception that the amount of 2-methylpentane-2,4-diol is 35 g and the amount of sodium hydroxide is 30 g (35 wt% solution). ).

Product: 175 g translucent, stable emulsion which can be further diluted to 30% with soft water.

Example 4

All were carried out as in Example 2, except that the dilution with soft water was performed with 65 g (ml) of water.

Product: 120 g 66% stable resin emulsion.

Claims (2)

A process for the preparation of a stable hydrophilic resin emulsion by partial alkaline saponification of the resin, wherein the rosin resin having a melting point below 100 ° C or a rosin resin having a melting point of less than 20% by weight is 20% by weight of resin. 50% by weight of C 4 -C 8 alkylene diol at 70-95 ° C in a molten atmosphere, preferably under a stream of nitrogen, with 25-35% by weight of the resin being 30-50% by weight of the resin. aqueous alkali metal hydroxide solution and then 15-25% by weight of urea are added, followed by the preparation of an aqueous emulsion of 30-70% by weight of water, preferably softened water, at a temperature of 50-60 ° C. 2. A process according to claim 1 wherein the alkylene diol is 2-methylpentane-2,4-diol.