CN1238434C - Preparation method of brucite, limestone superfine powder - Google Patents

Abstract

The present invention relates to a preparation method for the superfine powder of brucite and limestone. Brucite, limestone powder, a dispersing agent and a processing agent are used for being once ground at 50 DEG C to 150 DEG C to obtain superfine powder with a particle size which is smaller than 10 mu m. The present invention has the material adding proportion that 0.10 to 3.50 shares of the dispersing agent and 0.30 to 3.30 shares of the processing agent are added into every hundred shares of the brucite and the limestone powder, and the total adding amount of the dispersing agent and the processing agent is 1.00 to 5.50 shares. The dispersing agent is one or two kinds of white oil, polyocarboxy acid and polyols, and the use amounts of the white oil, the polyocarboxy acid and the polyols are respectively 0.00 to 3.33 shares, 0.00 to 3.00 shares and 0.00 to 3.000 shares. Compared with the prior art, the cost of the present invention is obviously lowered. The superfine powder of brucite and limestone is added into a macromolecular material, and a flame-retardant grade material with an oxygen index above 29 can be obtained. The cheap superfine powder and a superfine additive product of a magnesium oxide can be supplied to a fire retardant market.

Description

Brucite, Wingdale ultrafine powder preparation method

Technical field

What the present invention relates to is to be the technology of preparing of the ultrafine powder of raw material with natural brucite, Wingdale, particularly makes with breaking method.

Background technology

Fire retardant in the macromolecular material can delay fire spreading in fire.But some traditional fire retardant can decomposite toxic gas in big fire, and the personnel that cause poison and polluted air.The magnesium hydroxide of heavy and lime carbonate at high temperature decompose water outlet and carbonic acid gas, can play cooling effect and calcium, magnesium oxide do not fire and comes into one's own.Natural crystal brucite, Wingdale (calcite) are ideal fire retardants comparatively, and being added to needs these raw materials to become atomic little particle just to be unlikely and to influence the performance that it had originally, pulverize the primary study work that just becomes this work in the macromolecular material.This respect has had not little progress in recent years.Its method is broadly divided into dry method, wet method, does and wet-milling bonded three classes.CN1095080AC (application number 93111803.4) is that the laggard promoting the circulation of qi stream of raw material heat is pulverized multistage static separation, this dry ground legal system superfine heavy calcium carbonate fineness, whiteness, purity and active aspect all very good, but it is many to take off not open the inherent facility investment of conventional air breaking method institute, energy consumption is big, the defective of operative technique complexity can be made into active water-ground limestone micropowders as add promoting agent in raw material.Wet grinding research is more: as CN1042522C (ZL94104018.6) is to grind the back with amides flocculation and dehydration, solves muddy and is difficult to filtering problem, and its main technique is roughing, fine grinding, slagging-off, flocculation dewatering etc.; CN1039402 (ZL95108710.X) adds the sodium polyacrylate dispersion agent to carry out three grades of sand millings; CN1356361A (application number 01142497.4) adds poly-carbonyl acid type dispersion agent, fatty acid metal salt grinding water magnesite or sintered magnesia in water.CN1056166C (ZL96102845.9) then is that first dry ground sizes mixing that dispersion, wet ultra-fine grinding, chemical stability are handled, drying.Wet grinding can obtain more fine-grained magnesium hydroxide, lime carbonate, but will be through filter dehydration and drying process to make powdered product, because the small-particle in the mud has bigger cohesion tendency, the dry back utmost point gives caking.

Summary of the invention

At the defective that above-mentioned prior art exists, the present invention aims to provide a kind of simple, cheap and effectively prepare the processing method of ultra-fine powdery brucite or Wingdale.

The present invention adopts the good grinding machine of efficient, when grinding, add dispersion agent in case reunion that occurs in the crushing process and bonding phenomenon take place, add treatment agent simultaneously particle surface is carried out hydrophobic treatment, grind the ultrafine powder that obtains by disposable dry grinding, satisfy the requirement of good dispersity in the macromolecular material.

Concrete preparation method is, requires natural brucite or Wingdale raw material to reach 200～300 order fineness, adds in the shredder, adds dispersion agent and treatment agent simultaneously, grinds at 50～150 ℃ to form next time.The dispersion agent dosage is that the raw material of per 100 weight adds 0.10～4.00 weight, with 0.30～3.00 weight for well; The treatment agent dosage is 0.30～3.30 weight, and for well, and the reinforced total amount of dispersion agent and treatment agent is 1.00～5.50 weight with 0.50～2.60 weight, with 1.20～5.00 for well.Dispersion agent is 1 in white oil, polyocarboxy acid type dispersion agent, the polyvalent alcohol dispersion agent or 2 kind, and its dosage is respectively 0.00～3.00 weight, 0.00～3.50 weight, 0.00～3.50 weight; With 0.17～2.60,0.03～3.30,0.30～3.00 for well.Treatment agent is 1 in titanic acid ester, aluminic acid ester, the silane finish or 2 kind, and its dosage is respectively 0.00～3.30 weight, 0.00～3.00 weight, 0.00～3.00 weight, with 0.07～3.00,0.03～2.60,0.03～2.50 for well.

Used dispersion agent, treatment agent all are existing, can buy in market, comprise polyacrylic salt or ester as the polyocarboxy acid type dispersion agent, the salt of alkene and toxilic acid or ester copolymerization, the copolymerization of alkene and acrylate or salt etc., divided amount＜5000, be advisable with 1000～2000.Polyvalent alcohol is a propylene glycol, glycerine, trolamine.Titanic acid ester also is that market is on sale, as isopropyl triisostearoyl titanate; sec.-propyl three stearyl-titanic acid ester; three oleoyl isopropyl titanates; three (dodecyl benzenesulfonyl) isopropyl titanate; isopropyl tri (dioctylphosphato)titanate; sec.-propyl three (dodecyl tetradecyl) titanic acid ester; sec.-propyl two (dodecyl tetradecyl) methacryloyl titanic acid ester; sec.-propyl dodecyl tetradecyl dimethyl allene acyl titanate; sec.-propyl distearyl ylmethyl acryl titanic acid ester; isopropyl tri (dioctylpyrophosphato)titanate; sec.-propyl three (dibutyl pyrophosphoric acid ester acyl group) titanic acid ester; two (dioctylphyrophosphoric acid ester acyl group) chloro ethanoyl titanic acid ester; two isostearoyl base oxo ethanoyl titanic acid ester; two (dibutyl pyrophosphoryl oxygen base) oxo ethanoyl titanic acid ester.

Silane has:

γ-(methacrylic acyloxy) propyl trimethoxy silicane (A174), chloropropyltrimethoxy silane, γ-(1,2-encircles propoxy-) propyl trimethoxy silicane (A187), vinyl three (beta-methoxy-oxyethyl group) silane (A172), vinyltrimethoxy silane, γ-propyl methacrylate Trimethoxy silane, γ-glycidyl ether propyl trimethoxy silicane etc.The trade mark that photochemical plant produced is set in Nanjing commonly used is KH-540,570,580 product.

The main model of aluminic acid ester:

DL-411-A, DL-411-AF, DL-411-D, DL-411-DF, DL-411-B, DL-411-C, DL-811, DL-412-A, DL-42-B, DL-812, DL-414, DL-451-A, DL-851 etc.

Use aforesaid method, no matter be brucite or lime carbonate, can be easy to obtain the following ultrafine powder of 10 μ m, add to and can obtain oxygen index in the macromolecular material and be higher than 29 flame retardant grade material, and the mechanical property of macromolecular material is fine, can satisfy the requirement of fire retardant and additive on rubber and the plastics fully.

Compared with prior art, remove surface modification in its dry grinding technology, separation circuit, drying process, the cumbersome step of pulverizing process again from, greatly simplify technology, production cost obviously reduces, for fire retardant market and additive market provide cheap heavy magnesium hydroxide and calcium carbonate superfine powder.

Embodiment

For universal description characteristics of the present invention more, especially exemplified by following numerical example.Raw material is 200～300 purpose brucite and Paris whites.

Per 100 weight breeze feeding quantity (weight)		Example
															1	2	3	4	5	6	7	8	9	10	11	12	13
		The breeze kind		M	M	M	M	M	M	M	M	M	M	C														C	C
Dispersion agent	White oil														1.30	0.17		0.70	2.60								0.70
		Poly carboxylic acid			3.30 A	0.03 A	0.30 A	0.50 A			1.40 B	0.13 A	0.50 B															0.30 A
	Polyvalent alcohol															0.83 N					0.70 N	3.00 O				0.70 N
		Treatment agent	Metatitanic acid fat	3.00	1.30	1.70	0.50		1.70		1.30	0.07		0.70															2.00
Aluminic acid lipoprotein																0.03 Q		2.67 Q		1.70 R		1.00 R			1.30 S
			Silane								0.03 X		2.50 Y
Grinding temperature ℃															70	90	100	100	100	100	100	100	140	140	100	90			80
		Milling time h

Annotate: M is a brucite, and C is a Wingdale

A: sodium polyacrylate B: polyethylene sodium maleate N: trolamine O: propylene glycol

Q：DL-411-A R：DL-411B S：DL-412A X：KH-540 Y：KH-58

All brucite or ultra-fine branches of Wingdale through grinding play particle diameter less than 10 μ m, and such ultrafine powder is added in the macromolecular material, can obtain oxygen index and be higher than 29 flame retardant grade material.

Claims (3)

1, the preparation method of a kind of brucite, Wingdale ultrafine powder, it is characterized by brucite, limestone powder and dispersion agent, treatment agent 50～150 ℃ grind next time and the ultrafine powder of particle diameter＜10 μ m; Raw material brucite powder, the limestone powder that its reinforced proportioning is per 100 weight adds the dispersion agent of 0.10～4.00 weight and the treatment agent of 0.30～3.30 weight, and it is 1.00～5.50 weight that dispersion agent and treatment agent add total amount;

Wherein, described raw material brucite powder, its fineness of limestone powder are 200～300 orders;

Described dispersion agent is in white oil, polyocarboxy acid type dispersion agent, the polyvalent alcohol dispersion agent 1～2 kind, and its used weight is respectively 0.00～3.00,0.00～3.50,0.00～3.50; Wherein polyocarboxy acid type dispersant molecule amount is＜5000 the polyacrylic salt or salt or the multipolymer of ester or the multipolymer of alkene and acrylic acid salt or ester of ester, alkene and toxilic acid; The polyvalent alcohol dispersion agent is propylene glycol, glycerine or trolamine;

Described treatment agent is 1～2 kind in titanic acid ester, aluminic acid ester and the silane, and its used weight is respectively 0.00～3.30,0.00～3.00,0.00～3.00;

A kind of as in vibrating ball mill, ball mill, rod mill, the sand mill of the equipment that described grinding is used.

2, according to the preparation method of the described brucite of claim 1, Wingdale ultrafine powder, it is characterized by 100 weight brucite powders, limestone powder adds the dispersion agent of 0.30～3.00 weight and the treatment agent of 0.50～2.60 weight, it is 1.20～5.00 weight that dispersion agent and treatment agent add total amount;

Wherein said dispersion agent white oil, polyocarboxy acid type dispersion agent, the used weight of polyvalent alcohol dispersion agent are respectively 0.17～2.60,0.03～3.30,0.30～3.00;

Described treatment agent titanic acid ester, aluminic acid ester and the used weight of silane are respectively 0.07～3.00,0.03～2.60,0.03～2.50.

3, the preparation method of brucite according to claim 1 and 2, Wingdale ultrafine powder, the polyocarboxy acid type that it is characterized by in the dispersion agent is a sodium polyacrylate, polyalcohols is a trolamine.