CN105968877A - Preparation method of hydromagnesite packing filled with unsaturated polyester resin - Google Patents

Preparation method of hydromagnesite packing filled with unsaturated polyester resin Download PDF

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Publication number
CN105968877A
CN105968877A CN201610593369.7A CN201610593369A CN105968877A CN 105968877 A CN105968877 A CN 105968877A CN 201610593369 A CN201610593369 A CN 201610593369A CN 105968877 A CN105968877 A CN 105968877A
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China
Prior art keywords
mixed
agent solution
polyester resin
unsaturated polyester
hydromagnesite
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CN201610593369.7A
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Chinese (zh)
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CN105968877B (en
Inventor
郑水林
田海山
刘立新
贾立新
叶鹏
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Jiangsu Xibeili New Material Co ltd
China University of Mining and Technology Beijing CUMTB
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Jiangsu Xibeili New Material Co ltd
China University of Mining and Technology Beijing CUMTB
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02Compounds of alkaline earth metals or magnesium
    • C09C1/028Compounds containing only magnesium as metal
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Macromonomer-Based Addition Polymer (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

The invention discloses a preparation method of hydromagnesite packing filled with unsaturated polyester resin. The preparation method comprises the steps that hydromagnesite powder and titanium dioxide are compounded according to the mass ratio (95-98):(2-5) of the hydromagnesite powder to titanium dioxide to obtain compound powder; polyethylene glycol and triethanolamine are mixed according to the mass ratio (1-3):(1-3) of polyethylene glycol to triethanolamine and then fully stirred and mixed to be uniform by adding water to be prepared into a mixed modifying agent solution with the mass concentration of 25%-50%; the compound powder and the mixed modifying agent solution are weighed separately according to the mass ratio 100:(2-8) of the compound powder to the mixed modifying agent solution and synchronously metered and fed into continuous powder surface modifying equipment to be subjected to organic surface modifying treatment at the temperature of 70 DEG C-110 DEG C. According to the method, the hydromagnesite packing which is good in compatibility with the unsaturated polyester resin, high in whiteness and low in cost can be obtained by compounding the hydromagnesite powder and titanium dioxide and conducting organic surface modifying through the mixed modifying agent.

Description

A kind of basic magnesite filler preparation method filling unsaturated polyester resin
Technical field
The present invention relates to a kind of basic magnesite filler preparation method filling unsaturated polyester resin, belong to mineral material and add Work and applied technical field.
Background technology
Inorganic powder filled unsaturated polyester resin composite material is with unsaturated polyester resin as base material, and inorganic particle is Filler, adds a certain proportion of auxiliary agent, mix by stirring, pour, be gelled, one that the operation such as solidification is made novel organic/ Inorganic compounding building and ornament materials.This composite is referred to as " artificial stone ".Owing to having safe and environment-friendly, no color differnece, color The feature such as adjustable, is widely used in the indoor top grade decoration of hotel, office building, house etc..Unsaturated polyester resin is filled Inorganic particle filler can play enhancing product strength, reduce the effect such as shrinkage factor, reduction cost.
Basic magnesite is a kind of natural hydrated basic magnesium carbonate mineral, and chemical composition is 4MgCO3·Mg(OH)2·4H2O, It it is the high-quality magnesium ore resources originating in China's Tibetan Salt Lakes.Basic magnesite initial decomposition temperature, between 220-240 DEG C, decomposes and produces Solid MgO be overlying on combustible surface and play the effect of fire-retardant oxygen barrier, the flue dust that burning produces can also be adsorbed simultaneously, reduce cigarette Density;Decompose the gas H produced2O and CO2Around fuel gas and the concentration of oxygen can be diluted;The heat that decomposition reaction absorbs The temperature of surrounding can be reduced, so basic magnesite can be as inorganic fire-retarded filler.It addition, basic magnesite quality is pure Only, color and luster is pure white, and impurity content is low, and the basic magnesite powder body obtained after super-fine processing has good transparent and higher Whiteness.Filling unsaturated polyester resin with hydromagnesite stone powder for filler, prepared organic/inorganic composite decorative building material has The features such as decomposition temperature is high, smoke density is little, product cost is low.
Summary of the invention
On the basis of existing technology, the invention provides a kind of basic magnesite filler system filling unsaturated polyester resin Preparation Method, by hydromagnesite stone ore after broken, grinding and surface organic modification, can obtain and the unsaturated polyester resin compatibility Good, whiteness basic magnesite filler higher, lower-cost.
The technical solution used in the present invention: a kind of basic magnesite filler preparation method filling unsaturated polyester resin, main Comprise the following steps that:
(1) by hydromagnesite stone powder: hydromagnesite stone powder is compounded by the mass ratio of titanium dioxide=95-98:2-5 with titanium dioxide, To composite granule;
(2) Polyethylene Glycol is pressed: Polyethylene Glycol is mixed by the mass ratio of triethanolamine=1-3:1-3 with triethanolamine, then adds water It is thoroughly mixed uniformly, is configured to the mixed and modified agent solution that mass concentration is 25-50%;
(3) by composite granule: the mass ratio of mixed and modified agent solution=100:2-8 weighs composite granule and mixed and modified respectively Agent solution, and synchronous measurement feeds in continuous powdery surface modifying apparatus, carries out surface organic at a temperature of 70-110 DEG C Modification.
Optimizing further, described in step (1), the particle size distribution of hydromagnesite stone powder is d50=2-8 μm, d90=20-70 μm, dmax=60-120μm。
Optimizing further, titanium dioxide described in step (1) is the answering of any one or both in rutile-type, anatase titanium dioxide Closing, whiteness is not less than 95%.
Optimizing further, in step (3), the mass ratio of composite granule and mixed and modified agent solution is specially composite granule: Mixed and modified agent solution=100:3-6.
Optimizing further, continuous powdery surface modifying apparatus described in step (3) is that the continuous powder surface of SLG type changes Property machine.
Hydromagnesite stone powder is compounded with titanium dioxide by the present invention, utilizes high whiteness and the high covering power of titanium dioxide, can To improve the whiteness of basic magnesite filler further.After the blended modifying agent of hydromagnesite stone powder carries out surface organic modification, it is inhaled Oil value significantly reduces, and enhances the compatibility between unsaturated polyester resin.So, in the present invention, the basic magnesite of preparation is filled out Material is filled in unsaturated polyester resin, and loading is uniformly dispersed greatly and easily, and the composite obtained has good fire-retardant Performance and mechanical property, compared with the most conventional filling aluminium hydrate, the unsaturated polyester resin that basic magnesite filler is filled Heat stability improve, the production cost of product declines to a great extent.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme and technique effect are described in detail, but the present invention Scope be not restricted to specific examples below.
In example 1 below-6, continuous powdery surface modifying apparatus used is the continuous powder surface of SLG-3/300 Modifying machine;The oil factor of basic magnesite filler is detected according to the method in standard GB/T/T 3780.4-2008;Use DN-B2 The whiteness of whiteness instrument detection basic magnesite filler.
First, preparation is for hydromagnesite stone powder used in embodiment 1-6: original ore size is less than the basic magnesite of 300mm Raw ore uses after jaw crusher coarse crushing, then feed kibbler roll in small, broken bits to granularity less than 20mm;Then, LHJ type whirlpool is fed Rotating mechanical shock formula pulverizing grading machine, grinding reaches d to particle size distribution50=5.0μm、d90=57μm、dmax=90 μm, i.e. obtain Hydromagnesite stone powder for embodiment 1-6.
Embodiment 1:(1) press hydromagnesite stone powder: the mass ratio of titanium dioxide=95:5, weigh hydromagnesite stone powder 285kg, titanium White lead 15kg compounds, and obtains composite granule 300kg;(2) press Polyethylene Glycol: the mass ratio of triethanolamine=1:3, weigh Polyethylene Glycol 0.9 kg, triethanolamine 2.7kg mix, and then add water and are thoroughly mixed uniformly, are configured to mass concentration It is the mixed and modified agent solution 9kg of 40%;(3) composite granule is pressed: the mass ratio of mixed and modified agent solution=100:3, will be compound Powder body 300kg, mixed and modified agent solution 9kg synchronous measurement feed in continuous powdery surface modifying apparatus, the temperature of 90 DEG C Under carry out surface organic modification process.After surface organic modification processes, the oil factor of detection basic magnesite filler is 0.25ml/ G, whiteness is 88%.
Embodiment 2:(1) press hydromagnesite stone powder: the mass ratio of titanium dioxide=96:4, weigh hydromagnesite stone powder 288kg, titanium White lead 12kg compounds, and obtains composite granule 300kg;(2) press Polyethylene Glycol: the mass ratio of triethanolamine=3:1, weigh Polyethylene Glycol 2.7kg, triethanolamine 0.9kg mix, and then add water and are thoroughly mixed uniformly, and being configured to mass concentration is The mixed and modified agent solution 12kg of 30%;(3) composite granule is pressed: the mass ratio of mixed and modified agent solution=100:4, by composite powder Body 300kg, mixed and modified agent solution 12kg synchronous measurement feed in continuous powdery surface modifying apparatus, at a temperature of 80 DEG C Carry out surface organic modification process.After surface organic modification processes, the oil factor of detection basic magnesite filler is 0.24ml/g, Whiteness is 87%.
Embodiment 3:(1) press hydromagnesite stone powder: the mass ratio of titanium dioxide=98:2, weigh hydromagnesite stone powder 294kg, titanium White lead 6kg compounds, and obtains composite granule 300kg;(2) press Polyethylene Glycol: the mass ratio of triethanolamine=2:3, weigh poly- Ethylene glycol 1.8kg, triethanolamine 2.7kg mix, and then add water and are thoroughly mixed uniformly, and being configured to mass concentration is The mixed and modified agent solution 9kg of 50%;(3) composite granule is pressed: the mass ratio of mixed and modified agent solution=100:3, by composite powder Body 300kg, mixed and modified agent solution 9kg synchronous measurement feed in continuous powdery surface modifying apparatus, at a temperature of 110 DEG C Carry out surface organic modification process.After surface organic modification processes, the oil factor of detection basic magnesite filler is 0.23ml/g, Whiteness is 85%.
Embodiment 4:(1) press hydromagnesite stone powder: the mass ratio of titanium dioxide=97:3, weigh hydromagnesite stone powder 291kg, titanium White lead 9kg compounds, and obtains composite granule 300kg;(2) press Polyethylene Glycol: the mass ratio of triethanolamine=2:1, weigh poly- Ethylene glycol 2.0 kg, triethanolamine 1.0 kg mix, and then add water and are thoroughly mixed uniformly, and being configured to mass concentration is The mixed and modified agent solution 12kg of 25%;(3) composite granule is pressed: the mass ratio of mixed and modified agent solution=100:4, by composite powder Body 300kg, mixed and modified agent solution 12kg synchronous measurement feed in continuous powdery surface modifying apparatus, at a temperature of 70 DEG C Carry out surface organic modification process.After surface organic modification processes, the oil factor of detection basic magnesite filler is 0.26ml/g, Whiteness is 86%.
Embodiment 5:(1) press hydromagnesite stone powder: the mass ratio of titanium dioxide=96:4, weigh hydromagnesite stone powder 288kg, titanium White lead 12kg compounds, and obtains composite granule 300kg;(2) press Polyethylene Glycol: the mass ratio of triethanolamine=1:2, weigh Polyethylene Glycol 2kg, triethanolamine 4kg mix, and then add water and are thoroughly mixed uniformly, and being configured to mass concentration is 40% Mixed and modified agent solution 15 kg;(3) composite granule is pressed: the mass ratio of mixed and modified agent solution=100:5, by composite granule 300kg, mixed and modified agent solution 15kg synchronous measurement feed in continuous powdery surface modifying apparatus, at a temperature of 100 DEG C Carry out surface organic modification process.After surface organic modification processes, the oil factor of detection basic magnesite filler is 0.22ml/g, Whiteness is 87%.
Embodiment 6:(1) press hydromagnesite stone powder: the mass ratio of titanium dioxide=95:5, weigh hydromagnesite stone powder 285kg, titanium White lead 15kg compounds, and obtains composite granule 300kg;(2) press Polyethylene Glycol: the mass ratio of triethanolamine=1:1, weigh Polyethylene Glycol 2.7kg, triethanolamine 2.7kg mix, and then add water and are thoroughly mixed uniformly, and being configured to mass concentration is The mixed and modified agent solution 18kg of 30%;(3) composite granule is pressed: the mass ratio of mixed and modified agent solution=100:6, by composite powder Body 300kg, mixed and modified agent solution 18kg synchronous measurement feed in continuous powdery surface modifying apparatus, the temperature of 100 DEG C Under carry out surface organic modification process.After surface organic modification processes, the oil factor of detection basic magnesite filler is 0.21 Ml/g, whiteness is 88%.
Above-described embodiment is not limitation of the present invention, and those of ordinary skill that this area is relevant is not it should be clear that Multiple modification or replacement, the technical side of all equivalents can also be had in departing from the basic inventive concept of the present invention and the situation of scope Case also should comprise within the scope of the present invention.The scope of patent protection of the present invention is as the criterion with the restriction of claim.

Claims (5)

1. fill a basic magnesite filler preparation method for unsaturated polyester resin, mainly comprise the following steps that:
(1) by hydromagnesite stone powder: hydromagnesite stone powder is compounded by the mass ratio of titanium dioxide=95-98:2-5 with titanium dioxide, To composite granule;
(2) Polyethylene Glycol is pressed: Polyethylene Glycol is mixed by the mass ratio of triethanolamine=1-3:1-3 with triethanolamine, then adds water It is thoroughly mixed uniformly, is configured to the mixed and modified agent solution that mass concentration is 25-50%;
(3) by composite granule: the mass ratio of mixed and modified agent solution=100:2-8 weighs composite granule and mixed and modified respectively Agent solution, and synchronous measurement feeds in continuous powdery surface modifying apparatus, carries out surface organic at a temperature of 70-110 DEG C Modification.
A kind of basic magnesite filler preparation method filling unsaturated polyester resin the most according to claim 1, its feature It is: described in step (1), the particle size distribution of hydromagnesite stone powder is d50=2-8 μm, d90=20-70 μm, dmax=60-120μm。
A kind of basic magnesite filler preparation method filling unsaturated polyester resin the most according to claim 1, its feature It is: titanium dioxide described in step (1) is any one in rutile-type, anatase titanium dioxide or both is compound, and whiteness is not less than 95%。
A kind of basic magnesite filler preparation method filling unsaturated polyester resin the most according to claim 1, its feature It is: in step (3), the mass ratio of composite granule and mixed and modified agent solution is specially composite granule: mixed and modified agent solution= 100: 3-6。
A kind of basic magnesite filler preparation method filling unsaturated polyester resin the most according to claim 1, its feature It is: continuous powdery surface modifying apparatus described in step (3) is the continuous powder surface modifier of SLG type.
CN201610593369.7A 2016-07-26 2016-07-26 A kind of basic magnesite filler preparation method for filling unsaturated polyester resin Expired - Fee Related CN105968877B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101418139A (en) * 2007-10-25 2009-04-29 中国地质大学(北京) Magnesium hydroxide/TiO2 composite material with flame resistance property and pigment
CN102627788A (en) * 2011-11-29 2012-08-08 中国矿业大学(北京) Surface modifier formula for significantly reducing calcium carbonate oil absorption value
CN102888020A (en) * 2012-09-24 2013-01-23 陈旭 Preparation method for brucite inorganic flame retardant

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101418139A (en) * 2007-10-25 2009-04-29 中国地质大学(北京) Magnesium hydroxide/TiO2 composite material with flame resistance property and pigment
CN102627788A (en) * 2011-11-29 2012-08-08 中国矿业大学(北京) Surface modifier formula for significantly reducing calcium carbonate oil absorption value
CN102888020A (en) * 2012-09-24 2013-01-23 陈旭 Preparation method for brucite inorganic flame retardant

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