CN109535482A - A kind of no resin, nano flame retardant masterbatch of binder free and preparation method thereof - Google Patents

A kind of no resin, nano flame retardant masterbatch of binder free and preparation method thereof Download PDF

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Publication number
CN109535482A
CN109535482A CN201811341521.8A CN201811341521A CN109535482A CN 109535482 A CN109535482 A CN 109535482A CN 201811341521 A CN201811341521 A CN 201811341521A CN 109535482 A CN109535482 A CN 109535482A
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CN
China
Prior art keywords
nanometer
flame retardant
brucite powder
agent
powder
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Pending
Application number
CN201811341521.8A
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Chinese (zh)
Inventor
孙忠祥
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Sub-Safe Scientific And Technological Novel Material Limited-Liability Co In Dalian
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Sub-Safe Scientific And Technological Novel Material Limited-Liability Co In Dalian
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Priority to CN201811341521.8A priority Critical patent/CN109535482A/en
Publication of CN109535482A publication Critical patent/CN109535482A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/20Compounding polymers with additives, e.g. colouring
    • C08J3/22Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/223Packed additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2217Oxides; Hydroxides of metals of magnesium
    • C08K2003/2224Magnesium hydroxide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

Abstract

A kind of no resin, nano flame retardant masterbatch of binder free and preparation method thereof.When preparation: firstly, nanometer brucite powder is added in the modifying machine of continuous powdery surface, mist sprays into the depolymerizing agent after diluting.Nanometer brucite powder is sufficiently broken up depolymerization, drying and surface and coats one layer of depolymerizing agent, and the nanometer brucite powder of surface active is prepared.Then, by the nanometer brucite powder of surface active, it is sent into the processing that degasser carries out removing air and increases activation nanometer brucite powder product density.Finally, by treated, modified Nano brucite powder feeding dry type roll-in granulator is pelletized.Nano flame retardant masterbatch produced by the invention is free of binder and resin, therefore loading is high, versatility is good, effective component is high.And masterbatch good dispersion, compression strength is big, yield is high, and low energy consumption, since powder is flown upward in effective solution use process, the problem of bring all has a significant impact to worker's health and workshop condition.

Description

A kind of no resin, nano flame retardant masterbatch of binder free and preparation method thereof
Technical field
The invention belongs to the technologies of preparing of fire retardant, in particular to the system without resin, the nano flame retardant masterbatch of binder free Preparation Method and application.
Technical background
Nano level flame retardant powder is due to nano effect, compared with conventional flame retardant, has excellent performance.
However, nanometer powder surface hydrophilic oleophobic, easy reunion is difficult to directly apply, it is necessary to by surface treatment.In table In terms of surface treatment, used at present is that wet mixing is legal, i.e., first mixes nano flame retardant powder, surface treating agent and a large amount of solvent Stirring is closed, fire-retardant slurries are made.Then fire-retardant slurries are filtered, obtains fire-retardant powder filter cake.Filter cake is after pulverizer crushes Obtain smashed fire retardant wet cake.Wet cake crushes break up again, after can finally obtaining surface treatment after drying Nano flame retardant powder.The legal complex process of wet mixing, production cycle length, high production cost.
And nano-powder is easy to produce dust, to worker's health and workshop condition in production and process All have a great impact.Current solution is that masterbatch is made in nano material.But the method has certain defect, such as carries Body resin must be consistent with final resin, and the lubricating system in conventional masterbatch must match with final resin, otherwise easily Cause the sharp fall of fire proofing physical and chemical performance.Further, since material used in the plastic product client of downstream is a variety of Multiplicity, therefore flame-retardant master batch manufacturer will also convert basis material when doing masterbatch to solve the problems, such as compatibility, very It is cumbersome.
In terms of granulation, it is currently used have squeeze out tie rod water cooling, fervent water cooling, earnestly air-cooled or screw extruder (it is single/ It is double) carry out the technologies such as extrusion granulator.These granulation techniques needs are handled raw material under conditions of vacuum compression or heating, Production technology is complicated, and the production cycle is longer, high production cost.And the peculiar smell that high temperature generates plastics is big, and electricity consumption is big, worker Large labor intensity.The masterbatch especially produced since through extrusion process, brittleness is big, dust is more, and dispersion effect is general, The demand for not only being well positioned to meet production, using, but also many troubles are brought to daily production and application.
In order to solve these problems, the present invention does not add resin, binder and lubricant in pelletization, therefore fills Amount is high, versatility is good, effective component is high.And it can reduce cost.
The present invention carries out surface activation process to the fire-retardant powder of nanoscale using depolymerizing agent, can effectively avoid fire-retardant mother After material is added in matrix resin, nanometer grade powder cannot uniformly be distributed to the problems in matrix resin because of hard aggregation.
Nano flame retardant powder is activated using continuous powdery surface modifying machine, can play and coat on one side, one Frontier defense stops the effect of nanometer powder polymerization.The hard aggregation of nanoscale fire proofing can effectively be prevented.
The present invention uses dry-mixing cladding process, and depolymerizing agent is uniformly coated on nano flame retardant powder surface.It is closed with wet mixing Cladding process is compared, and dry-mixing cladding process is low containing quantity of solvent in whole process due to using continuous powdery surface modifying machine, therefore Powder is completed while not needing filtering, crush, is dry, crushing the multiple steps broken up again, but coat in modifying machine Drying, break up depolymerization, one step of whole process can be completed.This greatly simplifies technical process, and reduce energy and disappear Consumption, entire production process is without discharge, whole process closing, without dust pollution.The requirement of green, energy-saving and environmental protection can be reached.
Flame-retardant master batch is made in the fire-retardant powder of nanoscale, can be effectively solved " the frame generated during production application Bridge " phenomenon.It is of special importance that can be effectively solved in fire-retardant powder use process since powder is flown upward, bring is to work The problem of human body health and workshop condition all have a significant impact.And powder can be reduced to fly upward, to the wear problem of equipment.
It is pelletized using dry type roll-in granulator, with short production cycle, simple process, granulation product compression strength is big, produces Amount is big, does not generate secondary environmental pollution.And with conventional extrusion tie rod water cooling, fervent water cooling, earnestly air-cooled or Screw Extrusion Machine (mono-/bis -) granulation is compared, and is not needed to heat using dry type roll-in granulation mechanism grain, can be effectively reduced energy consumption.
Summary of the invention
It is an object of the invention to solve above-mentioned technical problem, it is female to provide a kind of no resin, the nano flame retardant of binder free Material and preparation method thereof.
The technical solution adopted by the invention is as follows:
A kind of no resin, binder free nano flame retardant masterbatch by nanometer brucite powder 92%-99.3%, depolymerizing agent 0.6%-3%, diluent 0.1-5% composition.
The depolymerizing agent is that coupling agent and dispersing agent compound, and wherein the additive amount of coupling agent is nano flame retardant masterbatch The 0.5%-2% of gross mass, the additive amount of dispersing agent are the 0.1%-1% of nano flame retardant masterbatch gross mass.
The coupling agent is vinyltriethoxysilane, γ-amine propyl-triethoxysilicane, N- β amine ethyl-γ amine One of propyl-triethoxysilicane, polyamides amine silane or a variety of mixtures.
The dispersing agent is Sodium Polyacrylate, polyvinyl alcohol, neopelex, odium stearate, lauroyl two One of ethanol amine, tetradecyl chloride amido propyl dimethyl benzyl amine or a variety of mixtures.
The diluent is one of water, ethyl alcohol or isopropanol or a variety of mixtures.
The method without resin, the nano flame retardant masterbatch of binder free, step are as follows:
(1) it prepares depolymerizing agent: coupling agent and dispersing agent is configured to depolymerizing agent in proportion.Wherein the additive amount of coupling agent is The 0.5%-2% of nano flame retardant masterbatch gross mass, the additive amount of dispersing agent are the 0.1%-1% of nano flame retardant masterbatch gross mass.
(2) surface active nanometer brucite powder: nanometer brucite powder is added in the modifying machine of continuous powdery surface, misty Depolymerizing agent after diluting is sprayed into, wherein nanometer brucite powder is 92%-99.3%, depolymerizing agent 0.6%-3%, and diluent is The nanometer brucite powder of surface active is prepared in 0.1-5%;
(3) the nanometer brucite powder of surface active degasser is sent into carry out removing air and increase to activate nanometer shepardite The processing of powder bulk density;
(4) by treated, modified Nano brucite powder feeding dry type roll-in granulator is pelletized, and no tree is prepared The nano flame retardant masterbatch of rouge, binder free.
Beneficial effects of the present invention:
1. using dry-mixing cladding process, depolymerizing agent is uniformly coated on nano flame retardant powder surface.It closes and coats with wet mixing Method is compared, and dry-mixing cladding process is low containing quantity of solvent in whole process due to using continuous powdery surface modifying machine, therefore is not required to The dry of powder is completed while filtering, crush, drying, crushing the multiple steps broken up again, but coating in modifying machine It is dry, break up depolymerization, one step of whole process can be completed.This greatly simplifies technical process, and reduce energy consumption, whole A production process is without discharge, whole process closing, without dust pollution.The requirement of green, energy-saving and environmental protection can be reached.
2. being activated using continuous powdery surface modifying machine to nanometer brucite powder, it can play and coat on one side, The effect for preventing nanometer powder from polymerizeing on one side.The hard aggregation of nanometer brucite powder can effectively be prevented.
3. carrying out surface activation process to nanometer brucite powder using depolymerizing agent, effectively flame-retardant master batch can be avoided to add After into matrix resin, nanometer grade powder cannot uniformly be distributed to the problems in matrix resin because of hard aggregation.
4. being pelletized using dry type roll-in granulator, with short production cycle, simple process, granulation product compression strength is big, Yield is big, does not generate secondary environmental pollution.And it is squeezed with conventional extrusion tie rod water cooling, fervent water cooling, earnestly air-cooled or screw rod Machine (mono-/bis -) granulation out is compared, and is not needed to heat using dry type roll-in granulation mechanism grain, can be effectively reduced energy consumption.
5. carrying out removing air before granulation to nanoscale flame-retardant master batch, increasing the pretreatment of density, not only contribute to Improve powder feeding efficiency, it is often more important that, the generation of bubble in manufactured masterbatch is advantageously reduced, and then be conducive to improve masterbatch Compression strength.
6. not adding resin and binder in pelletization, therefore loading is high, versatility is good, effective component is high.And It can reduce cost.
7. flame-retardant master batch is made in the fire-retardant powder of nanoscale, it can be effectively solved and generated during production application " bridge formation " phenomenon.It is of special importance that can be effectively solved in fire-retardant powder use process since powder is flown upward, for workshop The problem of environment, worker's health all have a great impact.
Specific embodiment
Embodiment 1
(1) it prepares depolymerizing agent: 1kg coupling agent and 1kg dispersing agent uniformly being mixed, depolymerizing agent is made.
(2) surface active nanometer brucite powder: 95kg nanometers of brucite powders are added in the modifying machine of continuous powdery surface, Mist sprays into depolymerizing agent of the 5kg after diluting, and wherein depolymerizing agent is 2kg, and receiving for surface active is prepared in diluent 3kg Rice brucite powder;
(3) the nanometer brucite powder of surface active degasser is sent into carry out removing air and increase to activate nanometer shepardite The processing of powder bulk density;
(4) by treated, modified Nano brucite powder feeding dry type roll-in granulator is pelletized, and no tree is prepared The nano flame retardant masterbatch of rouge, binder free.

Claims (5)

1. the nano flame retardant masterbatch of a kind of no resin, binder free, it is characterised in that: prepared by mass percentage by following components It forms: nanometer brucite powder 92%-99.3%, depolymerizing agent 0.6%-3%, diluent 0.1-5%.
2. the nano flame retardant masterbatch of a kind of no resin according to claim 1, binder free, it is characterised in that: described Depolymerizing agent is that coupling agent and dispersing agent compound, and wherein the additive amount of coupling agent is the 0.5%- of nano flame retardant masterbatch gross mass 2%, the additive amount of dispersing agent is the 0.1%-1% of nano flame retardant masterbatch gross mass.
3. the nano flame retardant masterbatch of a kind of no resin according to claim 2, binder free, it is characterised in that: described Coupling agent is vinyltriethoxysilane, γ-amine propyl-triethoxysilicane, N- β amine ethyl-γ amine propyl-triethoxysilicane One of alkane, polyamides amine silane or a variety of mixtures;The dispersing agent is Sodium Polyacrylate, polyvinyl alcohol, dodecane One of base benzene sulfonic acid sodium salt, odium stearate, lauroyl diethanolamine, tetradecyl chloride amido propyl dimethyl benzyl amine are more The mixture of kind.
4. nano flame retardant masterbatch according to claim 1 or 2 or 3, it is characterised in that: the diluent is water, ethyl alcohol Or one of isopropanol or a variety of mixtures.
5. the preparation method of any nano flame retardant masterbatch of claim 1-4, it is characterised in that step are as follows:
(1) it prepares depolymerizing agent: coupling agent and dispersing agent is configured to depolymerizing agent in proportion.Wherein the additive amount of coupling agent is nanometer The 0.5%-2% of flame-retardant master batch gross mass, the additive amount of dispersing agent are the 0.1%-1% of nano flame retardant masterbatch gross mass.
(2) surface active nanometer brucite powder: nanometer brucite powder is added in the modifying machine of continuous powdery surface, and mist sprays into Depolymerizing agent after diluting, wherein nanometer brucite powder is 92%-99.3%, depolymerizing agent 0.6%-3%, diluent 0.1- 5%, the nanometer brucite powder of surface active is prepared;
(3) the nanometer brucite powder of surface active degasser is sent into carry out removing air and increase to activate nanometer brucite powder The processing of product density;
(4) by treated, modified Nano brucite powder feeding dry type roll-in granulator is pelletized, and no resin, nothing is prepared The nano flame retardant masterbatch of binder.
CN201811341521.8A 2018-11-12 2018-11-12 A kind of no resin, nano flame retardant masterbatch of binder free and preparation method thereof Pending CN109535482A (en)

Priority Applications (1)

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Application Number Priority Date Filing Date Title
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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1865335A (en) * 2006-06-26 2006-11-22 李彦波 High concentration plastic nano flame-proof agglomerate production method
CN1876730A (en) * 2006-06-09 2006-12-13 沈阳化工学院 Composite modifier surface modified brucite powder preparation method
CN102585327A (en) * 2011-12-30 2012-07-18 大连亚泰科技新材料有限公司 Functional master batch for low-smoke halogen-free fireproof aluminum-plastic plate
CN102653599A (en) * 2012-05-08 2012-09-05 大连盖特科技发展有限公司 Active magnesium flame retardant with high-molecule coupling agent and preparation method of active magnesium flame retardant
CN102888020A (en) * 2012-09-24 2013-01-23 陈旭 Preparation method for brucite inorganic flame retardant
CN103044710A (en) * 2012-12-28 2013-04-17 大连亚泰科技新材料股份有限公司 Method for preparing flame retardant from natural brucite and application of flame retardant in cable compound
KR20160124712A (en) * 2016-10-10 2016-10-28 규 재 유 The manufacturing method of magnesium hydroxide and calcium chloride using dolomite for raw material

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1876730A (en) * 2006-06-09 2006-12-13 沈阳化工学院 Composite modifier surface modified brucite powder preparation method
CN1865335A (en) * 2006-06-26 2006-11-22 李彦波 High concentration plastic nano flame-proof agglomerate production method
CN102585327A (en) * 2011-12-30 2012-07-18 大连亚泰科技新材料有限公司 Functional master batch for low-smoke halogen-free fireproof aluminum-plastic plate
CN102653599A (en) * 2012-05-08 2012-09-05 大连盖特科技发展有限公司 Active magnesium flame retardant with high-molecule coupling agent and preparation method of active magnesium flame retardant
CN102888020A (en) * 2012-09-24 2013-01-23 陈旭 Preparation method for brucite inorganic flame retardant
CN103044710A (en) * 2012-12-28 2013-04-17 大连亚泰科技新材料股份有限公司 Method for preparing flame retardant from natural brucite and application of flame retardant in cable compound
KR20160124712A (en) * 2016-10-10 2016-10-28 규 재 유 The manufacturing method of magnesium hydroxide and calcium chloride using dolomite for raw material

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Application publication date: 20190329

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