CN104194418A - Modified attapulgite with flame retardant property and preparation method thereof - Google Patents

Abstract

The invention discloses modified attapulgite with flame retardant property. The modified attapulgite is prepared from the following raw materials in parts by weight: 100-120 parts of attapulgite, 0.4-0.6 part of sodium citrate, 0.3-0.4 part of clove oil, 4-5 parts of sodium carbonate, 1-1.4 parts of ureidohydantoin, 0.4-0.6 part of polyether polyol, 5-7 parts of antimonous oxide, 0.4-0.6 part of manganese acetate, 1-2 parts of dimethyl terephthalate, 0.4-0.6 part of dimethyl carbonate, 0.2-0.4 part of fatty acid amide succinate disodium, a proper amount of water, 5-10 parts of an assistant and 30-40 parts of 8-10% hydrochloric acid solution. According to the attapulgite disclosed by the invention, the surface activity of the attapulgite is improved by means of an acid activation technology, and thus the attapulgite with high dispersion and high viscosity is prepared; the flame retardant property is improved due to addition of antimonous oxide; the viscosity of the attapulgite is improved by addition of dimethyl terephthalate and dimethyl carbonate; and the attapulgite is suitable for lots of fields such as packing of coatings, textile sizing materials and plastic rubber and is excellent in performance.

Description

A kind of have the attapulgite modified and preparation method thereof of flame retardant properties

Technical field

The invention belongs to attapulgite manufacture field, particularly a kind of have the attapulgite modified and preparation method thereof of flame retardant properties.

Background technology

Attapulgite is a kind of crystalloid hydrous magnesium aluminium silicate mineral, has unique layer chain-like structure feature, in its structure, has crystal lattice, Na+, the Ca2+, Fe3+, the Al3+ that in side crystal, contain non-quantitative, and crystal is needle-like, fibrous or fiber collection shape.Attapulgite has unique dispersion, high temperature resistant, the anti-good colloidal property such as saline and alkaline and higher adsorption bleaching ability.And there is certain plasticity-and cohesive force, and water-absorbent is strong, tool viscosity and plasticity-when wet, and dry post shrinkage is little, not quite aobvious crackle, water soaking collapses loose, and suspension is met not flocculation sediment of dielectric medium.Therefore attapulgite is widely used in the numerous areas such as sewage disposal, adsorption cleaning, washing composition, rubber, coating, papermaking, light industry, agricultural, makeup, is a kind of important nonmetallic minerals, the part but attapulgite also comes with some shortcomings.

In order further to improve the result of use of attapulgite, strengthen its whole physical and chemical performance, conventionally before use it is carried out to modification, improve the dispersing property of attapulgite, gel viscosity, colloidity, rheological property.And along with the development of industrial technology, also need to improve some other performances of attapulgite, as performances such as germ resistance, thixotropy, oilness, viscosity, suspension, adsorptivities, to meet the needs of different field development.

Summary of the invention

The object of the present invention is to provide a kind of the attapulgite modified and preparation method thereof of flame retardant properties that have, the surfactivity of this attapulgite is high, also has polymolecularity, high viscosity, fire-retardant feature.

Technical scheme of the present invention is as follows:

A kind of have the attapulgite modified of flame retardant properties, it is characterized in that being made by the raw material of following weight part: attapulgite 100-120, Trisodium Citrate 0.4-0.6, Syzygium aromaticum stem oil 0.3-0.4, sodium carbonate 4-5, wallantoin 1-1.4, polyether glycol 0.4-0.6, antimonous oxide 5-7, manganous acetate 0.4-0.6, dimethyl terephthalate (DMT) 1-2, methylcarbonate 0.4-0.6, fatty acid amide sulfo-succinic acid fat disodium 0.2-0.4, water are appropriate, auxiliary agent 5-10,8-10% hydrochloric acid soln 30-40;

Described auxiliary agent is made by the raw material of following weight part: nano-calcium carbonate 4-5, agalloch eaglewood essential oil 0.1-0.2, aminoresin 0.2-0.3, Hydroxylated acrylic resin 0.4-0.5, terminal carboxyl polyester resin 0.3-0.4, aluminum chloride 3-4, nano zeolite powder 1-2, silicone oil 0.1-0.2, molybdenumdisulphide 0.3-0.5, Strontium carbonate powder 0.1-0.2, boron nitride 0.1-0.2, precipitated chalk 1-2, Cellulose diacetate 0.1-0.2, bamboo fibers 2-3; Preparation method is: nano-calcium carbonate, precipitated chalk, nano zeolite powder, molybdenumdisulphide, Strontium carbonate powder, boron nitride, Cellulose diacetate, bamboo fibers mixed grinding is even, obtain mixed powder; By other remaining component mixing and stirring, with gained powder mixed grinding 20-30 minute, reheat to 60-70 ℃, griding reaction 30-40 minute, obtains again.

The described attapulgite modified preparation method with flame retardant properties, is characterized in that comprising the following steps:

(1) attapulgite is sent into calcining furnace, at 300-400 ℃, calcine 3-4 hour, take out and pulverize, cross 20 mesh sieves, add in the water of 340-380 weight part, under 100-200 rev/min, stir 10-12 hour, obtain attapulgite suspension, add 8-10% hydrochloric acid soln, be heated to 50-60 ℃, stir 1-2 hour, then add while stirring sodium carbonate to continue to stir 1-2 hour, filter, being washed to pH value is 6-8, refilter, dry, obtain activating attapulgite powder;

(2) other remaining components are added in residue water, stir, obtain slurry;

(3) to attapulgite powder, blow the warm air of 50-60 ℃ it is seethed, then spray into the slurry that (2) vaporific step obtains in the powder seething, after the two is fully mixed, maintenance temperature is 50-60 ℃, continues to seethe 30-40 minute;

(4) mixture (3) step being obtained is dried, and grinds to form the particle of 5-80 μ m, obtains.

Beneficial effect of the present invention

Attapulgite of the present invention has improved the surfactivity of attapulgite by acid activation technological approaches, thus prepared there is high dispersive, the attapulgite of high viscosity performance; By adding antimonous oxide, improved flame retardant properties; Dimethyl terephthalate (DMT), methylcarbonate, improved the viscosity of attapulgite; This attapulgite is applicable to the numerous areas such as the filler, textiles sizing agent, plastic, rubber of coating, excellent performance.

Embodiment

A kind of have the attapulgite modified of flame retardant properties, by following weight part (kilogram) raw material make: attapulgite 100-120, Trisodium Citrate 0.5, Syzygium aromaticum stem oil 0.4, sodium carbonate 4.5, wallantoin 1.2, polyether glycol 0.5, antimonous oxide 6, manganous acetate 0.5, dimethyl terephthalate (DMT) 1.5, methylcarbonate 0.5, fatty acid amide sulfo-succinic acid fat disodium 0.3, water are appropriate, auxiliary agent 8,9% hydrochloric acid soln 35;

Described auxiliary agent by following weight part (kilogram) raw material make: nano-calcium carbonate 4.5, agalloch eaglewood essential oil 0.1, aminoresin 0.2, Hydroxylated acrylic resin 0.5, terminal carboxyl polyester resin 0.3, aluminum chloride 3.5, nano zeolite powder 1.5, silicone oil 0.1, molybdenumdisulphide 0.4, Strontium carbonate powder 0.2, boron nitride 0.1, precipitated chalk 1.5, Cellulose diacetate 0.1, bamboo fibers 2.5; Preparation method is: nano-calcium carbonate, precipitated chalk, nano zeolite powder, molybdenumdisulphide, Strontium carbonate powder, boron nitride, Cellulose diacetate, bamboo fibers mixed grinding is even, obtain mixed powder; Again by other remaining component mixing and stirring, with gained powder mixed grinding 25 minutes, reheat to 65 ℃, griding reaction 35 minutes, obtains.

The described attapulgite modified preparation method with flame retardant properties, comprises the following steps:

(1) attapulgite is sent into calcining furnace, at 350 ℃, calcine 3.5 hours, take out and pulverize, cross 20 mesh sieves, add in the water of 360 weight parts, under 150 revs/min, stir 11 hours, obtain attapulgite suspension, add 9% hydrochloric acid soln, be heated to 55 ℃, stir 1.5 hours, then add while stirring sodium carbonate to continue to stir 1.5 hours, filter, being washed to pH value is 7, refilter, dry, obtain activating attapulgite powder;

(2) other remaining components are added in residue water, stir, obtain slurry;

(3) to attapulgite powder, blow the warm air of 55 ℃ it is seethed, then spray into the slurry that (2) vaporific step obtains in the powder seething, after the two is fully mixed, keeping temperature is 55 ℃, continues to seethe 35 minutes;

(4) mixture (3) step being obtained is dried, and grinds to form the particle of 5-80 μ m, obtains.

Experimental data:

The attapulgite modified specific surface area of the present embodiment is 287 ㎡/g, is added to the water by 4%, and tested viscosity is 14845.6mPa.s, dissolution time≤4min, and degree of discoloring >=24%, is 76% to kaolin simulated sewage turbidity removal rate.

Claims (2)

1. one kind has the attapulgite modified of flame retardant properties, it is characterized in that being made by the raw material of following weight part: attapulgite 100-120, Trisodium Citrate 0.4-0.6, Syzygium aromaticum stem oil 0.3-0.4, sodium carbonate 4-5, wallantoin 1-1.4, polyether glycol 0.4-0.6, antimonous oxide 5-7, manganous acetate 0.4-0.6, dimethyl terephthalate (DMT) 1-2, methylcarbonate 0.4-0.6, fatty acid amide sulfo-succinic acid fat disodium 0.2-0.4, water are appropriate, auxiliary agent 5-10,8-10% hydrochloric acid soln 30-40;

Described auxiliary agent is made by the raw material of following weight part: nano-calcium carbonate 4-5, agalloch eaglewood essential oil 0.1-0.2, aminoresin 0.2-0.3, Hydroxylated acrylic resin 0.4-0.5, terminal carboxyl polyester resin 0.3-0.4, aluminum chloride 3-4, nano zeolite powder 1-2, silicone oil 0.1-0.2, molybdenumdisulphide 0.3-0.5, Strontium carbonate powder 0.1-0.2, boron nitride 0.1-0.2, precipitated chalk 1-2, Cellulose diacetate 0.1-0.2, bamboo fibers 2-3; Preparation method is: nano-calcium carbonate, precipitated chalk, nano zeolite powder, molybdenumdisulphide, Strontium carbonate powder, boron nitride, Cellulose diacetate, bamboo fibers mixed grinding is even, obtain mixed powder; By other remaining component mixing and stirring, with gained powder mixed grinding 20-30 minute, reheat to 60-70 ℃, griding reaction 30-40 minute, obtains again.

2. the attapulgite modified preparation method with flame retardant properties according to claim 1, is characterized in that comprising the following steps:

(1) attapulgite is sent into calcining furnace, at 300-400 ℃, calcine 3-4 hour, take out and pulverize, cross 20 mesh sieves, add in the water of 340-380 weight part, under 100-200 rev/min, stir 10-12 hour, obtain attapulgite suspension, add 8-10% hydrochloric acid soln, be heated to 50-60 ℃, stir 1-2 hour, then add while stirring sodium carbonate to continue to stir 1-2 hour, filter, being washed to pH value is 6-8, refilter, dry, obtain activating attapulgite powder;

(2) other remaining components are added in residue water, stir, obtain slurry;

(3) to attapulgite powder, blow the warm air of 50-60 ℃ it is seethed, then spray into the slurry that (2) vaporific step obtains in the powder seething, after the two is fully mixed, maintenance temperature is 50-60 ℃, continues to seethe 30-40 minute;

(4) mixture (3) step being obtained is dried, and grinds to form the particle of 5-80 μ m, obtains.