JPH01115445A - Dispersant composition - Google Patents

Abstract

PURPOSE:To prepare the title dispersant composition useful as various dispersants by adding formalin to the sulfonation product of the mixture of naphthalene and a styrene-maleic acid copolymer to condense the materials, and then neutralizing the condensate. CONSTITUTION:Naphthalene and a styrene-maleic acid copolymer are mixed, and the mixture is sulfonated. In this case, 100pts.wt. naphthalene is ordinarily mixed with 1-500pts.wt. styrene-maleic acid copolymer. Sulfonation is appropriately carried out at 150-180 deg.C and 0-5kg/cm<2>G pressure for 0.5-5hr. Formalin is added to the sulfonation product, and the materials are condensed to produce a dispersant composition. Condensation is appropriately carried out by adding 50-300pts.wt. water and 50-80pts.wt. formalin to 100pts.wt. sulfonation product.

Description

[Detailed Description of the Invention] C. Industrial Field of Application] This invention relates to a dispersant composition, specifically a dispersant for coal slurry, a dispersant for cement (cement bait, mortar or concrete dispersant), and a dispersant for dyes. The present invention relates to a dispersant composition useful as a dispersant for pigments, a dispersant for emulsion polymerization, a dispersant for sludge, etc., and prepared by an efficient method.

[Prior Art] Dispersing inorganic solid particles or organic fine substances in a specific medium is required in various fields. A dispersant is usually used to improve the dispersibility.

For example, salts of formalin condensates of naphthalene sulfonic acid and salts of sulfonated styrene-maleic acid copolymers are known as dispersants that improve the dispersibility of cement particles in water in mortar and concrete (Japanese Patent Application Laid-open No. 61-83662).

These dispersants may be used alone, but in most cases, they are used in combination. However,
Conventionally, in preparing the dispersant composition obtained by this blending, a salt of a formalin condensate of naphthalene sulfonic acid and a salt of a sulfonated styrene-maleic acid copolymer were separately manufactured and blended. ;.

[Problem that the invention seeks to solve]

An object of the present invention is to provide a dispersant composition prepared by a more efficient method by eliminating the conventional complexity of separately manufacturing and blending the two components.

[Means for Solving the Problem] As a result of various studies to achieve the above object, the inventor initially mixed glass 7-talene and styrene-maleic acid copolymer, and subjected this mixture to a reaction treatment. It has been found that a dispersant composition can be prepared by -
This invention was made based on this knowledge.

That is, according to this invention, naphthalene and styrene
A dispersant composition is provided by sulfonating a mixture with a maleic acid copolymer, adding formalin to the sulfonated product for condensation, and then neutralizing the mixture.

In this invention, first, naphthalene and a styrene-maleic acid copolymer are mixed, and this mixture is sulfonated. There is no particular restriction on the mixing ratio of both, but usually 1 to 500 parts by weight, preferably 10 to 100 parts by weight of styrene-maleic acid copolymer per 100 parts by weight of naphthalene.
Part by weight.

There are no particular restrictions on the styrene-maleic acid copolymer used, but it usually has a number average molecular weight of 500 to 2 ONO1, preferably 800 to 10,000, and the proportion of styrene units is 20 to 90 mol%, preferably 40 to 80. mole%
Preferably.

Sulfonation of this mixture is usually carried out by adding a sulfonating agent without using a solvent. As the sulfonating agent, commonly used sulfonating agents such as sulfuric acid, chlorosulfuric acid, fuming sulfuric acid, and sulfuric anhydride are used. This sulfonating agent is 50 parts by weight per 100 parts by weight of 7 grains.
~500 parts by weight, preferably 70-200 parts by weight are used. The sulfonating agent may be added all at once or may be added in portions.

There are no restrictions on the conditions for sulfonation, but usually 80 to 200
°C, preferably 150-180 °C temperature, 0-10
kg/cra”G 1 preferably O-5ky/cm
” at a pressure of 0.1-10 hours, preferably 0.5-10 hours.
A reaction time of 5 hours is sufficient.

In this invention, formalin is then added to the sulfonated product thus obtained for condensation.

In the condensation, 20 to 30 parts by weight of water, preferably 50 to 30 parts by weight, are added to 100 parts by weight of the sulfonated product.
If desired, 0 to 100 parts by weight, preferably 10 to 60 parts by weight of concentrated sulfuric acid are added, and 30 to 100 parts by weight, preferably 50 to 80 parts by weight of formalin are added thereto.

There are no special restrictions on the condensation conditions, but usually 60 to 15
Temperature of 0°C, preferably 80-130'O, 0-10
kg/cm2G, preferably 0-5 kg/cm”
G pressure is carried out for 0.5 to 20 hours, preferably for 1 to 5 hours.

In this invention, the condensation product thus obtained is neutralized to obtain the desired dispersant composition.

As the neutralizing agent, hydroxides of sodium, potassium, calcium, etc., carbonates, bicarbonates, ammonia, amines, etc. can be used.

There are no special restrictions on the conditions for neutralization, but usually 3
0-100'c, preferably 50-80'0 and 0.5-
A treatment time of 5 hours, preferably 1 to 3 hours is sufficient.

[Effect of the invention] According to the present invention, a dispersant composition is prepared very efficiently, and the obtained dispersant composition can be used as a dispersant for coal slurry, a dispersant for cement, a dispersant for dyes, and a dispersant for pigments. It can be effectively used as a wide variety of dispersants, such as emulsion polymerization dispersants, sludge dispersants, etc.

[Example] Next, the present invention will be explained in more detail by giving examples and usage examples.

Example 7 100g of grain and styrene-maleic acid copolymer C
Manufactured by ARCOchemica1, SMA-200
0゜number average molecular weight 1700, acid value 37011sIKOH
/ 9) After mixing 309 and raising the temperature of this mixture to 90'O, concentrated sulfuric acid 1209 was added as a sulfonating agent, and the mixture was then reacted at a temperature of 165° C. and normal pressure for 2 hours to perform sulfonation.

Next, 60 g of water and 40 y of concentrated sulfuric acid were added to the sulfonated product.
was added, and further 37% by weight of formalin 609 was added, and the mixture was reacted at 95° C. and normal pressure for 4 hours to perform condensation.

Finally, an emulsion containing 90 g of calcium hydroxide was added to the condensation product obtained in this way, the produced calcium sulfate was removed by filtration, and 130 g of a 30% by weight aqueous sodium hydroxide solution was added to the obtained filtrate. 2 at °C. , #, neutralization treatment was performed to obtain 650 g of a dispersant composition as a 35% by weight aqueous solution.

Use example 1 (Preparation and evaluation of coal slurry) Coal (produced in Australia) 2009 shown in Table 1, dispersant composition obtained in Example (35% by weight aqueous solution) 4.6
g and water 57; were mixed, and then wet-pulverized using a mortar grinder to prepare a coal slurry. 82.5% of crushed coal has a particle size of 200 mesh or less.
Met.

Table 1 This coal slurry was placed in a beaker and its viscosity at 20°C was measured using a B-type viscometer, and found to be 990 centipoise.

Further, the coal slurry is taken in a plastic container,
After standing for 24 hours, it was passed through a 16-mesh sieve.

The agglomeration rate was determined from the amount of coal slurry remaining in the container and the amount of coal slurry remaining on the sieve, and the stability of the coal slurry was confirmed, and the aggregation rate was extremely small at 6% by weight.

Agglomeration rate - Usage example 2 (Preparation and evaluation of concrete) Cement (manufactured by Tokuyama Soda Co., Ltd., ordinary, Portland cement) 460 kg/m'', fine aggregate (sand from Nagahama, Shikoku University Mishima, surface dry specific gravity 2.52, coarse Particle ratio 214) 673 kg7a
”.

Coarse aggregate (crushed stone from Suohanaoka, surface dry ratio g2.'IO1 coarse grain ratio 6.48, maximum dimension 20111111) l114&g
/m', 161 kg/m3 of water, and 1.01 g amount % (solid content based on cement) of the dispersant composition obtained in the example (35% by weight aqueous solution) were stirred and mixed using a forced mixer to prepare concrete.

The air content, slump value, and compressive strength after curing of this concrete were measured.

The results are shown in Table 2.

Table 2 *' JISA-1128 *'' JISA-1101 *3 JISA-1108 Usage Example 3 (Preparation and evaluation of inorganic pigment slurry) Heavy calcium carbonate (manufactured by Nitto Kofun Kasei Kogyo Co., Ltd., MS-
Zoo), 30 g of water, and 0.2% by weight (solid content based on heavy calcium carbonate) of the dispersant composition (35% by weight aqueous solution) obtained in the example were placed in a container and heated at 20°C.
After stirring and mixing for 1 minute at 20°C, the viscosity was measured using a B-type viscometer, and the viscosity at 20°C was as low as 120 centivoise.

Claims (1)

[Claims] A dispersant composition obtained by sulfonating a mixture of naphthalene and a styrene-maleic acid copolymer, adding formalin to the sulfonated product for condensation, and then neutralizing the mixture.