JP2002003793A - Method of producing rosin flake - Google Patents

Abstract

PROBLEM TO BE SOLVED: To economically produce rosin flakes that are useful as a starting material for surfactant with excellent antiblocking properties. SOLUTION: In this method of producing rosin flakes, the rosin acid ester in the rosin are neutralized with an inorganic alkali whereby the softening point is largely raised by the partial formation of rosin acid salt and the antiblocking properties are increased.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a high-quality and economical production of rosin flakes having excellent blocking resistance and useful as a raw material for a surfactant.

[0002]

2. Description of the Related Art An aqueous solution of an alkali salt of rosin and stabilized rosin in which rosin is disproportionated or hydrogenated (hereinafter, these rosins are simply referred to as rosin) is used as an emulsifier for polymerizing synthetic rubber and synthetic resin and an air entrainer for concrete. It is widely used as a surfactant. The aqueous solution of an alkali salt of rosin is produced by dissolving rosin crushed into blocks in heated alkaline water. Conventionally, in this manufacturing process,
Since rosin cannot be flaked because its softening point is as low as about 80 ° C., solid rosin packed in an iron drum is used. The operation of cutting open the drum and breaking the removed rosin into blocks with a hammer or crusher involves considerable danger. In addition, since a large amount of rosin fine powder is scattered, it is indispensable for workers to wear environmental protection such as eyes, mouths, feet, hands, etc., and to install a powerful exhaust device to take environmental measures.

[0003]

SUMMARY OF THE INVENTION An object of the present invention is to solve the dangers involved in taking out rosin from a drum having a filling amount of 220 to 230 kg and a means for solving the problem of the working environment which is worsened by the scattering of a large amount of rosin fine powder. To provide.

[0004]

Means for Solving the Problems It has been known that operability and safety can be remarkably improved if the rosin packing can be switched from a drum-packed form to a paper bag or a flake containing flexible container. Since the softening point of rosin is as low as about 80 ° C. and blocking easily occurs, it has not been commercialized so far. Therefore, as a result of intensive research to solve this problem, the formation of a partial inorganic alkali salt in rosin greatly increased the softening point and improved the blocking resistance to a practical level, resulting in flakes. Was found to be possible. Further, at present, the water-soluble alkali salts of rosin produced in large quantities are potassium salts and sodium salts, but the alkali salt aqueous solution produced by the rosin flakes according to the present invention using the same inorganic alkali can be produced by a conventional method. There was no change in quality from the manufactured one.

[0005] The rosin flakes of the present invention provide an application field used as an aqueous solution of an inorganic alkali salt of rosin, particularly a potassium salt and a sodium salt. For example, emulsifier for emulsion polymerization of synthetic rubber and synthetic resin, emulsifier for asphalt, air entrainer for concrete, emulsifier for pesticides,
Emulsifiers for adhesives and the like. When the rosin flake of the present invention is used in these fields, the same type of rosin salt is already partially formed, so that it is shorter than the conventional method,
A rosin salt aqueous solution can be produced safely without further deteriorating the working environment.

[0006] That is, the flake forming step of the present invention is incorporated as the last step in the production of rosin, disproportionated rosin, stabilized rosin, etc., and 20% to 50% of the rosin acid contained in the rosin is inorganic. A method for producing rosin flakes in which potassium rosin acid or sodium rosinate is formed by neutralization with an alkali, and the softening point of rosin is increased from about 80 ° C. to at least 100 ° C. to prevent blocking of flake pieces. It is.

[0007]

DESCRIPTION OF THE PREFERRED EMBODIMENTS The method of the present invention will be described below in detail. The rosin used in the present invention may be any of gum rosin, tall rosin and wood rosin, and may be a so-called stabilized rosin obtained by disproportionating or hydrogenating these. 180
By adding an inorganic alkali to rosin heated and melted at a temperature of from 230C to 230C, a potassium or sodium rosinate can be formed. As the inorganic alkali, caustic potash, caustic soda, potassium carbonate, sodium carbonate and the like are suitable. The addition amount of the inorganic alkali is preferably an amount that neutralizes 20% to 50% of the rosin acid in the rosin. If it is less than 20%, the softening point will not be sufficiently increased, and if it is more than 50%, the viscosity of the molten rosin will increase and it will be difficult to transport it through piping. The temperature at which neutralization is performed by adding an inorganic alkali is preferably from 180 ° C to 230 ° C. At 180 ° C. or lower, there is a risk of crystallization and loss of fluidity. At 230 ° C. or higher, rosin is easily colored and is not economically advantageous.
The neutralization reaction is completed within one hour. Subsequently, it is introduced into the flaker at the same temperature. The type of the breaker can be either a belt type or a drum type. The obtained rosin flake has a softening point of 100 ° C. or higher and does not cause blocking at a temperature of 40 ° C. or lower and can maintain a smooth flake state.

[0008]

The present invention will be described more specifically with reference to examples. Example 1 Acid value (KOHmg / g) in 100 L SUS dissolution tank
76 kg of molten disproportionated rosin at 220 ° C. having properties of 161, hue (Gardner color number) 6, and softening point of 78 ° C. are prepared. To this, 3.9 kg of caustic cauliflake, which neutralizes 32% of the rosin acid, was added over 30 minutes. The generated neutralized water was distilled out. Analysis after one hour revealed an acid value of 114, a hue of 6, and a softening point of 105 ° C. The temperature of the rosin was lowered to 180 ° C. and then introduced into the flaker. The obtained flakes were packed in a paper bag at a filling amount of 20 kg, stored under a constant temperature room at 40 ° C. for 60 days under a load of 100 g / cm ² corresponding to 20-stacking, but no blocking was observed. Furthermore, as a result of preparing an aqueous solution having a concentration of 25% and a pH of 10.5, which is a general use form, using the flakes, the dissolution time of rosin was about 20% as compared with the case of preparing from a conventional disproportionated rosin. In addition to the shortening, the color tone (Gardner color number) of the aqueous solution was exactly equal to 4, and there was no inferiority in transparency. The contents of dehydroabietic acid, which is the main component of the various rosin acids contained in rosin, and abietic acid, which affects the emulsion polymerization reaction, did not change at all before and after the flake forming step.

Example 2 In Example 1, caustic cauli flakes were replaced with rosin acid 4
The same operation as in Example 1 was performed except that the amount was changed to 5.5 kg, which is an amount for neutralizing 5%. As a result, the resulting partially neutralized rosin had a hue of 6, an acid value of 89, and a softening point of 113 ° C.
Met. When this rosin flake was tested under the same conditions of weight, temperature and duration as in Example 1, no blocking was observed.

Example 3 220 having properties of an acid value of 172, a hue of 6, and a softening point of 81 ° C.
70 kg of molten gum rosin at a temperature of 70 ° C. was prepared. To this, 4.6 kg of granular sodium carbonate neutralizing 40% of rosin acid is added to 30 parts.
Added over minutes. Analysis after 2 hours revealed an acid value of 10
3, hue 7, softening point 112 ° C. When the obtained flakes were tested under the same conditions of weight, temperature and period as in Example 1, no blocking was observed.

Comparative Example The disproportionated rosin used in Example 1 for comparison was 180 ° C.
So, I just flaked it. A blocking test was performed under the same conditions as in Example 1. As a result, about half of the blocks were blocked on the third day and aggregated into one lump. Therefore, the weight was reduced by half to 50 g / cm ² and the temperature was further reduced to 30 g / cm ^2.
The test was carried out at a temperature of 5 ° C., but almost the same blocking occurred on the fifth day.

[0012]

According to the present invention, rosin flakes having a significantly increased softening point and improved blocking resistance to a practical level can be produced. In the field where the rosin flakes of the present invention can be used, the working environment is greatly improved, which greatly contributes to cost reduction.

Claims (3)

[Claims] 1. A method for producing rosin flakes, wherein 20% to 50% of rosin acid contained in rosin is neutralized with an inorganic alkali. 2. The rosin is a gum rosin, a tall rosin, a wood rosin, or a stabilized rosin obtained by hydrogenating or disproportionating these rosins.
Of producing the described rosin flakes 3. The method for producing rosin flakes according to claim 1, wherein the rosinate partially neutralized with an inorganic alkali is potassium rosinate or sodium rosinate.