CN106882826A - A kind of preparation method of flame retardant of magnesium hydroxide - Google Patents
A kind of preparation method of flame retardant of magnesium hydroxide Download PDFInfo
- Publication number
- CN106882826A CN106882826A CN201510937275.2A CN201510937275A CN106882826A CN 106882826 A CN106882826 A CN 106882826A CN 201510937275 A CN201510937275 A CN 201510937275A CN 106882826 A CN106882826 A CN 106882826A
- Authority
- CN
- China
- Prior art keywords
- magnesium hydroxide
- flame retardant
- preparation
- magnesium
- filter cake
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/22—Magnesium hydroxide from magnesium compounds with alkali hydroxides or alkaline- earth oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Fireproofing Substances (AREA)
Abstract
The invention discloses a kind of preparation method of flame retardant of magnesium hydroxide, in turn include the following steps：After relevant temperature is heated to the magnesium chloride solution of magnesium chloride, to the compound precipitantses for adding calcium oxide, magnesia, NaOH to be formed after mixing with water in solution, after precipitating reagent to be composite is added completely, washing, filtering, magnesium hydroxide filter cake is obtained, furthermore, magnesium hydroxide filter cake is starched into treatment again；Finally, the magnesium hydroxide crushing grinding after treatment will be again starched, flame retardant of magnesium hydroxide is obtained.Magnesium hydroxide purity in obtained flame retardant of magnesium hydroxide of the invention is more than or equal to 99.0%, and flame retardant effect is excellent and product sequence is simple, with low cost, be adapted to industrialized production.
Description
Technical field
The present invention relates to field of fine chemical, more particularly to a kind of preparation method of flame retardant of magnesium hydroxide.
Background technology
There is within 1907 synthesis macromolecule phenolic resin, indicate opening for mankind's application synthesis macromolecular material
Begin.At present, macromolecular material is together with metal material, Inorganic Non-metallic Materials, as science and technology
With the important materials in economic construction.Especially in recent decades, plastics, rubber, synthetic fibers etc. gather
Compound material and its product are flourished, and they just replace rapidly traditional steel, metal, cement
And the natural polymer such as timber, cotton, it is widely used in each of the national economy such as industry, agricultural, military affairs
Department.But because macromolecular material is mainly made up of elements such as carbon, hydrogen, oxygen, most of polyphosphazene polymers
Compound belongs to flammable, combustible material, and in burning, HRR is big, and calorific value is high, flame propagation velocity
Hurry up, be difficult to extinguish, also produce thick smoke sometimes and toxic gas, the harm to environment is caused, to people's
There is huge threat in life security.Therefore, synthetic polymer and natural polymerses how to be improved
The anti-flammability of material has turned into a problem for urgent need to resolve.
Fire retardant refers to the flame retardancy that can improve combustibles or combustible, prevents material from being ignited and suppress fire
A kind of important auxiliary agent that flame spreads, holds fire hazardous, it is ensured that synthetic material makes macromolecular material is solved
Security aspect plays an important role.Wherein, during flame retardant of magnesium hydroxide is halogen-free flame retardants
One of most widely used kind.It is also steady with suppression cigarette, heat because magnesium hydroxide is while fire-retardant
It is qualitative, promote the characteristic such as base material incarbonization and acid scavenging capacity, be widely used in polyvinyl chloride (PVC),
Polypropylene (PP), polyethylene (PE), vinylacetate (EVA), polystyrene (PS), polyamide (PA) etc. are moulded
In material, elastomer and elastomeric material.Preferable magnesium hydroxide flame retardant profit be added in polymer require to have compared with
Purity and suitable size distribution high.Because magnesium hydroxide needs loading higher as fire-retardant profit,
If the particle of magnesium hydroxide used is larger, it is added to obtained composite in matrix, in hydroxide
Crackle is easily formed between magnesium and matrix, so as to influence the overall performance of material.And the purity of magnesium hydroxide
One of determinant of composite electric property, thus preferably magnesium hydroxide as fire-retardant filler its
Product purity, each element content, particle size range size etc. have demand higher.
The method of production magnesium hydroxide mainly has two kinds at present：One is the direct comminuting method of shepardite；Two is to contain
Magnesium raw material reacts conversion method.Because natural brucite purity is relatively low, macromolecule material is added to as fire retardant
The decline of composite electric property is frequently can lead in material.And contain magnesium raw material conversion method can by control
Different reaction conditions, prepares the flame retardant of magnesium hydroxide product of different size, therefore as production at present
The main method of flame retardant of magnesium hydroxide.Using the main of using in the prior art containing magnesium raw material transformation approach
Precipitating reagent is NaOH, ammoniacal liquor, milk of lime.Because independent NaOH and ammoniacal liquor are used as precipitating reagent,
Products obtained therefrom cost price is higher, so it is precipitating reagent that people increasingly tend to the milk of lime that raw material is easy to get
To prepare magnesium hydroxide products.
The content of the invention
For prior art flame retardant of magnesium hydroxide preparation method products obtained therefrom purity it is not high enough, be prepared into
The problems such as this is higher, a kind of product purity of present invention offer is high, lower-cost flame retardant of magnesium hydroxide system
Preparation Method.
The purpose of the present invention is reached by following measures：A kind of preparation of flame retardant of magnesium hydroxide is provided
Method, in turn includes the following steps：After relevant temperature is heated to the magnesium chloride solution of magnesium chloride,
To the compound precipitantses for adding calcium oxide, magnesia, NaOH to be formed after mixing with water in solution, treat
After compound precipitantses are added completely, washing, filtering obtains magnesium hydroxide filter cake, furthermore, by hydroxide
Magnesium filter cake is starched treatment again；Finally, the magnesium hydroxide crushing grinding after treatment will be again starched, hydrogen-oxygen is obtained
Change magnesium fire retardant.
Further, the mass fraction of the magnesium chloride in the magnesium chloride solution is 30%.
Further, the heating-up temperature terminal is 50~80 DEG C, and preferred scheme is for heating-up temperature terminal
60℃。
Further, in the compound precipitantses, wherein the mass fraction of the calcium oxide is 10%, institute
It is 0.1% to state the mass fraction of NaOH, and the calcium oxide is 200: 1 with the mass ratio of magnesia
Further, the reaction condition of the precipitation reaction is lasting isothermal reaction 60min at 60 DEG C.
Further, it is described to starch reaction again, the volume ratio of the volume of reactor and the magnesium chloride solution
It is 3~5: 1.
Further, the physics break process is that will again starch the magnesium hydroxide filter cake after treatment a diameter of
Re-dry after 60min is ground in the circulation ball mill of the zirconium oxide of 1mm~1.2mm.
Beneficial effect：Flame retardant of magnesium hydroxide of the invention and preparation method thereof is by the solution containing magnesium ion
It is middle to add by calcium oxide, magnesia, NaOH and the mixed compound precipitantses of water, then by control
Rational process conditions obtain purity flame retardant of magnesium hydroxide higher, are confirmed through many experiments, the hydrogen
The purity of magnesia fire retardant be more than or equal to 99.0%, and the preparation technology have yield it is high, prepare
The advantage of low cost.
Specific embodiment
Below by embodiment, the present invention is described in detail.
After relevant temperature is heated to the magnesium chloride solution of magnesium chloride, in solution add calcium oxide,
The compound precipitantses that magnesia, NaOH are formed after mixing with water, after precipitating reagent to be composite is added completely,
Washing, filtering, obtains magnesium hydroxide filter cake, furthermore, magnesium hydroxide filter cake is starched into treatment again；Most
Afterwards, the magnesium hydroxide crushing grinding after treatment will be again starched, flame retardant of magnesium hydroxide is obtained.
Further, the mass fraction of the magnesium chloride in the magnesium chloride solution is 30%.
Further, the heating-up temperature terminal is 50~80 DEG C, and preferred scheme is for heating-up temperature terminal
60℃。
Further, in the compound precipitantses, wherein the mass fraction of the calcium oxide is 10%, institute
It is 0.1% to state the mass fraction of NaOH, and the calcium oxide is 200: 1 with the mass ratio of magnesia
Further, the reaction condition of the precipitation reaction is lasting isothermal reaction 60min at 60 DEG C.
Further, it is described to starch reaction again, the volume ratio of the volume of reactor and the magnesium chloride solution
It is 3~5: 1.
Further, the physics break process is that will again starch the magnesium hydroxide filter cake after treatment a diameter of
Re-dry after 60min is ground in the circulation ball mill of the zirconium oxide of 1mm~1.2mm.
Embodiment
The magnesium chloride solution for adding 500mL mass fractions to be 8% in the reactor of 2L is warming up to
60 DEG C, compound precipitantses, the calcium oxide quality point of the compound precipitantses are added with the flow of 20ml/min
Number is 15%, and the mass fraction of NaOH is 0.1%, and calcium oxide is 200 with the mass ratio of magnesia:
1, compound precipitantses addition for needed for magnesium ion is precipitated completely theoretical amount 98.5%, it is described compound heavy
Shallow lake agent continues isothermal reaction 45min washing and filterings at 60 DEG C again after adding completely, treats in filtrate without chlorine
Untill ion, magnesium hydroxide filter cake is starched treatment again, obtained magnesium hydroxide slurry so that after starching again
Magnesium hydroxide slurry concentration be 40%, then in the circulation ball mill of the zirconium oxide of a diameter of 1mm
Grinding 60min is dried.
Above content is the further description done to the present invention with reference to optimal technical scheme, it is impossible to recognized
The specific implementation of fixed invention is only limitted to these explanations.To general technical staff of the technical field of the invention
For, on the premise of design of the invention is not departed from, simple deduction can also be made and replaced, all
Protection scope of the present invention should be considered as.
Claims (7)
1. a kind of preparation method of flame retardant of magnesium hydroxide, it is characterised in that in turn include the following steps：Will
After being heated to relevant temperature with the magnesium chloride solution of magnesium chloride, in solution add calcium oxide, magnesia,
The compound precipitantses that NaOH is formed after mixing with water, after precipitating reagent to be composite is added completely, washing,
Filtering, obtains magnesium hydroxide filter cake, furthermore, magnesium hydroxide filter cake is starched into treatment again；Finally, will
The magnesium hydroxide crushing grinding after treatment is starched again, obtains flame retardant of magnesium hydroxide.
2. the preparation method of a kind of flame retardant of magnesium hydroxide according to claim 1, it is characterised in that
The mass fraction of the magnesium chloride in the magnesium chloride solution is 30%.
3. the preparation method of a kind of flame retardant of magnesium hydroxide according to claim 1, it is characterised in that
The heating-up temperature terminal is 50~80 DEG C.
4. the preparation method of a kind of flame retardant of magnesium hydroxide according to claim 1, it is characterised in that,
In the compound precipitantses, wherein the mass fraction of the calcium oxide is 10%, the matter of the NaOH
Amount fraction is 0.1%, and the calcium oxide is 200: 1 with the mass ratio of magnesia.
5. the preparation method of a kind of flame retardant of magnesium hydroxide according to claim 1, it is characterised in that
The reaction condition of the precipitation reaction is lasting isothermal reaction 60min at 60 DEG C.
6. the preparation method of a kind of flame retardant of magnesium hydroxide according to claim 1, it is characterised in that
Described to starch reaction again, the volume ratio of the volume of reactor and the magnesium chloride solution is 3~5: 1.
7. the preparation method of a kind of flame retardant of magnesium hydroxide according to claim 1, it is characterised in that
The physics break process is that will again starch the magnesium hydroxide filter cake after treatment in a diameter of 1mm~1.2mm
Re-dry after 60min is ground in the circulation ball mill of zirconium oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510937275.2A CN106882826A (en) | 2015-12-15 | 2015-12-15 | A kind of preparation method of flame retardant of magnesium hydroxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510937275.2A CN106882826A (en) | 2015-12-15 | 2015-12-15 | A kind of preparation method of flame retardant of magnesium hydroxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106882826A true CN106882826A (en) | 2017-06-23 |
Family
ID=59174431
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510937275.2A Pending CN106882826A (en) | 2015-12-15 | 2015-12-15 | A kind of preparation method of flame retardant of magnesium hydroxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106882826A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109810487A (en) * | 2019-01-24 | 2019-05-28 | 中山市绿浪助剂有限公司 | Heat-resistant plastic |
| CN113150377A (en) * | 2020-10-16 | 2021-07-23 | 南通意特化工有限公司 | Preparation method of magnesium hydroxide flame retardant |
-
2015
- 2015-12-15 CN CN201510937275.2A patent/CN106882826A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109810487A (en) * | 2019-01-24 | 2019-05-28 | 中山市绿浪助剂有限公司 | Heat-resistant plastic |
| CN113150377A (en) * | 2020-10-16 | 2021-07-23 | 南通意特化工有限公司 | Preparation method of magnesium hydroxide flame retardant |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102502728B (en) | Magnesium hydroxide flame retardant and preparation method thereof | |
| CN102069519B (en) | Fire retardant for wood, and preparation method and treatment process thereof | |
| CN102321274B (en) | Hydrotalcite-ammonium polyphosphate halogen-free flame retardant and preparation method thereof | |
| CN104231539B (en) | A kind of process for dispersing of Graphene in phenolic resin and Graphene phenol-formaldehyde resin modified | |
| CN107304255B (en) | Composite flame-retardant agent, flame-retardant pitch and preparation method thereof | |
| CN111574751B (en) | Preparation method of modified melamine polyphosphate | |
| CN106882826A (en) | A kind of preparation method of flame retardant of magnesium hydroxide | |
| CN105037810A (en) | Method for preparing alginate modified brucite composite flame retardant | |
| CN101857692B (en) | PE/magnesium hydroxide composite flame retardant material | |
| CN102408625A (en) | Preparation method of composite material by using rare-earth doped hydrotalcite as halogen-free fire retardant and strengthening agent | |
| CN104183852B (en) | Phenolic resin-graphite-graphene composite battery bipolar grid plate and preparation method thereof | |
| CN106496920A (en) | low smoke density ABS resin and preparation method thereof | |
| CN109553891A (en) | A kind of environment friendly halogen-free fireproof cable material and preparation method thereof | |
| CN110054809B (en) | Composite flame retardant, preparation method thereof and application thereof in polypropylene | |
| CN110498951B (en) | ZIFs nanosheet/chitosan/kieselguhr hybrid and preparation method thereof | |
| CN102558691B (en) | Insulation rubber and preparation method thereof | |
| CN104262875A (en) | Intumescent flame-retardant cable material taking plant-based active carbon as synergist and preparation method thereof | |
| CN106554031A (en) | A kind of preparation method and flame retardant of magnesium hydroxide of flame retardant of magnesium hydroxide | |
| CN110128698A (en) | A kind of environmental-protection flame-retardant smoke suppressant and preparation method thereof | |
| CN109762253A (en) | A kind of high-strength anti-flaming polypropylene material | |
| CN101805619B (en) | Method for preparing nitrogen-phosphorus fire retardant | |
| CN110845779B (en) | Modified composite flame-retardant TPO resin and preparation method thereof | |
| CN103012851A (en) | Preparation method of superfine modified brucite flame retardant and application of superfine modified brucite flame-retardant to PVC (Polyvinyl Chloride) cable material | |
| CN103709589A (en) | Mica-ABS (Acrylonitrile Butadiene Styrene) flame-retardant insulation material and preparation method thereof | |
| CN104448546B (en) | A kind of catalytic flame retardancy mineral macromolecular material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170623 |
|
| WD01 | Invention patent application deemed withdrawn after publication |