CN107177200A - It is a kind of for additive of polymer and preparation method thereof - Google Patents
It is a kind of for additive of polymer and preparation method thereof Download PDFInfo
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- CN107177200A CN107177200A CN201710406650.XA CN201710406650A CN107177200A CN 107177200 A CN107177200 A CN 107177200A CN 201710406650 A CN201710406650 A CN 201710406650A CN 107177200 A CN107177200 A CN 107177200A
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- polymer
- additive
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5313—Phosphinic compounds, e.g. R2=P(:O)OR'
-
- 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
- C08K3/16—Halogen-containing compounds
-
- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
-
- 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
- C08K3/28—Nitrogen-containing compounds
-
- 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
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
-
- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/262—Alkali metal carbonates
-
- 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
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of additive for polymer, including：A：Phosphinates containing two substituted radicals, with following structural formula (I),Wherein, R1, R2It is identical or different, it is expressed as H, C1 C6 alkyl or C6 C18 aryl；M is Al；M is 3；B：Metal potassium element, wherein weight content of the metal potassium element in total additive are 10 450ppm.Additive preparation technology of the invention containing particular range content metal potassium element is simple, and production cost is low, and it is applied in polymer, can greatly improve the heat distortion temperature of combination of polymers Tetramune, and with efficient fire resistance.
Description
Technical field
The present invention relates to a kind of additive for polymer, and in particular to a kind of dioxane containing trace meter potassium element
Base phosphinates and preparation method thereof.
Background technology
Dialkylphosphinic salts, are widely used as fire retardant, it is known that it can be synthesized by different methods.Such as patent
DE4430932 discloses two substitution metal phosphinates and is used as fire retardant in polyester, and DE19910232, US6248921 two is specially
Profit discloses a kind of preparation method of two substitutions metal phosphinate.United States Patent (USP) US6359171B1 discloses a kind of dialkyl group
The preparation method of phosphinic acids aluminium, this method synthesizes monoalkyl phosphonate using yellow phosphorus first, then triggers second using free radical
Hydrolyzed after alkylene it is sour after with aluminium salt reaction obtain dialkyl phosphinic acid aluminium fire retardant.
Thermoplastic, because its excellent electrical property and processing characteristics are widely used in the row such as electronic apparatus, automobile, building
Industry, in order to meet flame-retardancy requirements and the environmental requirement of industry, generally meets material toward addition halogen-free flame retardants in thermoplastic
The above-mentioned requirements of material.
Dialkylphosphinic salts are high with bulk density as a kind of efficient halogen-free anti-inflaming agent, and amount of flame-retardant agent is small, machinery
Performance is good, and color and luster is good, and smoke density is low, the characteristics of CTI (phase ratio creepage tracking index) value is high, be widely used in polyamide, polyester,
In the thermoplasticity and thermosetting plastics such as unsaturated-resin, epoxy resin, polyurethane.
The present invention has been surprisingly found that through research, when containing trace meter potassium element in fire retardant dialkylphosphinic salts,
The higher fire resistance of polymer composition can not only be ensured, the thermal deformation of combination of polymers Tetramune can also be greatly improved
Temperature.
The content of the invention
It is an object of the invention to provide a kind of additive for polymer, the additive passes through in dialkyl phosphinic acid
Micro metal potassium element is added in salt, obtained polymer composition can be made to possess excellent fire resistance, and improve polymerization
The heat distortion temperature of compositions product.
Another object of the present invention is to provide a kind of preparation method of the above-mentioned additive for polymer.
The present invention is achieved by the following technical solutions：
A kind of additive for polymer, including：
A：Dialkylphosphinic salts, with following structural formula (I),
Wherein, R1, R2It is identical or different, it is expressed as H, C1-C6 alkyl or C6-C18 aryl, preferably ethyl, propyl group, fourth
Base, hexyl or cyclohexyl；
M is Al；M is 3；
B：Metal potassium element, wherein weight content of the metal potassium element in total additive are 10-450ppm.Preferred weight
Content is 20-350ppm, and more preferably weight content is 30-200ppm, and further preferred weight content is 40-100ppm.
The method of testing of the weight content of metal potassium element：0.05 ± 0.005g is taken to be used for the additive samples of polymer,
0.001g is accurate to, is put into micro-wave diminishing pot, 10mL is added and clears up acid in micro-wave diminishing pot, it is totally submerged sample
Product, slowly instill 1-2mL hydrogen peroxide, make sample and clear up acid reaction 1-2min, close the lid, sealed digestion tank, at 220 DEG C
Cleared up in convection oven, digestion time is 2h, after the completion of clearing up, take out counteracting tank, be cooled to room temperature, it is to be measured；If still had
Some particles are not cleared up, then slowly instill 1-2mL hydrogen peroxide repeat before clear up step, it is to be measured；If secondary do not clear up yet
Completely, it is necessary to which the settled solution that digestion solution is obtained after filtering is treats test sample, specifically, by the solution in micro-wave diminishing pot
It is transferred to 0.45 μm of filter membrane in volumetric flask, repeatedly rinses micro-wave diminishing pot with appropriate distilled water and be transferred to flushing liquor
In volumetric flask, then shaken up to graduation mark 50mL with distilled water diluting, it is to be measured；Using the complete of Agilent companies model 720ES
The weight content of metal potassium element, takes three surveys in automatic inductively coupled plasma atomic emission spectrometer analysis testing sample
The average out to final result of examination value.
The metal potassium element come from potassium-containing compound, the potassium-containing compound be selected from potassium chloride, potassium carbonate, potassium sulfate or
One or more in potassium nitrate.The source of metal potassium element pointed by the present invention is not limited only to the example above, no matter uses
The potassium-containing compound of which kind of form, can use atomic emission spectrometry to detect.The weight content of metal potassium element be with
Metal potassium element is in itself rather than on the basis of adding the potassium-containing compound of metal potassium element.The metallic potassium member represented with ppm
The weight content of element is calculated on the basis of gross weight of the present invention for the additive of polymer.
The polymer is polyester (such as PBT, PET), nylon (PA6, PA66), PPE, TPE, TPU or epoxy resin, excellent
Select nylon 6.
The present invention obtains being used to polymerize by the way that dialkyl hypophosphorous acid salt and potassium-containing compound is uniform in high-speed mixer and mixing
The additive of thing；
Wherein, one or more of the potassium-containing compound in potassium chloride, potassium carbonate, potassium sulfate or potassium nitrate.
The invention also discloses purposes of the above-mentioned additive for polymer as fire retardant.
The invention also discloses a kind of polymeric material for including the above-mentioned additive for polymer, including 5-25 weight
The additive for polymer of part, the polymer of 50-75 parts by weight or its mixture.
The polymer is polyester (PBT, PET), nylon (PA6, PA66 etc.), PPE, TPE, TPU or epoxy resin, preferably
For nylon 6.
Polymeric material of the present invention, can add different auxiliary agents, such as also wraps according to the different performance demand of material
Include the filler of 15-40 parts by weight and the auxiliary agent of 0.1-5 parts by weight.
The filler of the present invention is the material commonly used to reinforcing or filled polymer, it is possible to use two or more are inorganic to fill out
The mixture of material and/or reinforcing agent, preferably glass fibre.
The auxiliary agent can not disturb foregoing to wish property but improve the additional component of other beneficial properties, such as antioxygen
Agent, lubricant, releasing agent, nucleator, toner, light stabilizer.
The present invention compared with prior art, has the advantages that：
1) dialkylphosphinic salts containing particular range content metal potassium element that prepare of the present invention, as
The additive of polymer, the additive application can ensure the higher fire resistance of polymer composition in polymer, not only,
The heat distortion temperature of combination of polymers Tetramune can also be improved.
2) additive for polymer of the invention, preparation technology is simple, and production cost is low, is easy to large-scale production.
Embodiment
The present invention is further illustrated below by embodiment, following examples are the present invention preferably embodiment party
Formula, but embodiments of the present invention are not limited by following embodiments.
As described below now are done to raw material selected in embodiment and comparative example, but is not limited to these materials：
Component A dialkyl hypophosphorous acid aluminium：It is commercially available；Metal Determination of Potassium：Do not detect；
PA6：PA6M2000 (Meida Nylon Co., Ltd., Xinhui, Guangdong)；
Glass fibre：ECS301-HP (Chongqing Polycomp International Co., Ltd)；
Antioxidant：1010, (Jin Haiyabao)
Potassium-containing compound：It is commercially available
The method of testing of the weight content of metal potassium element of the present invention：0.05 ± 0.005g is taken to be used for adding for polymer
Plus agent sample, 0.001g is accurate to, is put into micro-wave diminishing pot, 10mL is added and clears up acid in micro-wave diminishing pot, make its complete
Full submergence sample, slowly instills 1-2mL hydrogen peroxide, makes sample and clear up acid reaction 1-2min, close the lid, sealed digestion
Tank, is cleared up in 220 DEG C of convection ovens, and digestion time is 2h, after the completion of clearing up, and is taken out counteracting tank, is cooled to room temperature, treats
Survey；If still there are some particles not clear up, then slowly instill 1-2mL hydrogen peroxide repeat before clear up step, it is to be measured；If two
It is secondary not clear up yet completely, it is necessary to the settled solution that digestion solution is obtained after filtering is treats test sample, specifically, by micro-wave digestion
Solution in tank is transferred in volumetric flask with 0.45 μm of filter membrane, and micro-wave diminishing pot is repeatedly rinsed with appropriate distilled water and will be rushed
Washing lotion is transferred in volumetric flask, then is shaken up with distilled water diluting to graduation mark 50mL, to be measured；Using Agilent companies model
The weight of metal potassium element contains in 720ES full-automatic inductively coupled plasma atomic emission spectrometer analysis testing sample
Amount, takes the average out to final result of three test values.
The heat distortion temperature of combination of polymers Tetramune of the present invention：The polymer contained in than polymer composition
Fusing point it is about high 20 DEG C at a temperature of by polymer composition injection moulding, manufacture thickness 0.5mm, width 10mm and long 30mm's
Piece.The piece is placed 100 hours in 40 DEG C, 95%RH (relative humidity) atmosphere gas.By the test film in infrared heating
In stove, in being heated at 150 DEG C 1 minute, then heated up with 100 DEG C/min of speed, the temperature that piece is deformed or is expanded is made
For the heat distortion temperature of composition article.
Combustibility of the present invention：UL94 Plastics Combustion performance tests；
UL 94 is determined for the test sample from every kind of polymer composition using thickness 1.5mm test sample to fire
Burn grade.It is below the defined burning grades of UL 94：
V-0：Batten is left after flame, and the sustained combustion time is no longer than 10s, 5 battens amount to continuing when lighting for 10 times
Burning time summation is no more than 50s, no molten drop drippage, flame without spreading to fixture phenomenon, sample light terminate after more than
Brightness burning time is no longer than 30s.
V-1：Batten is left after flame, and the sustained combustion time is no longer than 30s, 5 battens amount to continuing when lighting for 10 times
Burning time summation be no more than 250s, sample light terminate after twilight sunset burning time be no longer than 60s, other standards as
V-0。
V-2：Batten is left after flame, during sustained combustion, molten drop occurs, and molten drop can ignite absorbent cotton indicant,
Other same V-1 of standard.
Unclassified (ncl)：It is unsatisfactory for burning grade V-2.
Comparative example 1-2 (D1-D2) and embodiment 1-11 (B1-B11)
By the composition of the depicted of table 1, the component A and potassium-containing compound for weighing foregoing preparation are uniform in high-speed mixer and mixing, system
Obtain the additive of the invention for polymer.
Wherein, the present invention is by chemical combination containing potassium in preparation process for the additive metal Determination of Potassium of polymer
The actual interpolation amount of thing is adjusted and measured.
The comparative example 1-2 (D1-D2) of table 1 and embodiment 1-11 (B1-B11) additive for polymer
Comparative example 3-5, embodiment 12-22
Weighed by the proportioning in table 2 after each component is well mixed in high-speed stirred batch mixer and send into double screw extruder
In；Glass fibre is fed system by the side of double screw extruder and added, cold in a water bath through double screw extruder melting extrusion
But, granulate, produce polymer composition；And determine its UL-94 flame retardant rating and obtain polymer under foregoing test condition
Composition article simultaneously determines its heat distortion temperature, and specific test data is listed in Table 2 below.
The specific proportioning (parts by weight) and its test result respectively constituted in table 2 comparative example 3-5, embodiment 12-22
Claims (13)
1. a kind of additive for polymer, including：
A：Dialkylphosphinic salts, with following structural formula (I),
Wherein, R1, R2It is identical or different, it is expressed as H, C1-C6 alkyl or C6-C18 aryl；
M is Al；M is 3；
B：Metal potassium element, wherein weight content of the metal potassium element in total additive are 10-450ppm.
2. a kind of additive for polymer as claimed in claim 1, it is characterised in that the metal potassium element adds always
Plus the weight content in agent is 20-350ppm, preferred weight content is 30-200ppm, and more preferably weight content is 40-
100ppm。
3. a kind of additive for polymer as claimed in claim 1 or 2, it is characterised in that the weight of metal potassium element
The method of testing of content：Take 0.05 ± 0.005g to be used for the additive samples of polymer, be accurate to 0.001g, be put into micro-wave digestion
In tank, add 10mL and clear up acid in micro-wave diminishing pot, it is totally submerged sample, slowly instill 1-2mL hydrogen peroxide, make
Sample closes the lid, sealed digestion tank is cleared up, digestion time in 220 DEG C of convection ovens with clearing up acid reaction 1-2min
For 2h, after the completion of clearing up, counteracting tank is taken out, is cooled to room temperature, it is to be measured；If still there are some particles not clear up, then slowly instill 1-
2mL hydrogen peroxide clears up step before repeating, to be measured；If secondary do not clear up completely, it is necessary to by digestion solution after filtering yet
Obtained settled solution is treats test sample, specifically, the solution in micro-wave diminishing pot is transferred into capacity with 0.45 μm of filter membrane
In bottle, repeatedly rinse micro-wave diminishing pot with appropriate distilled water and flushing liquor is transferred in volumetric flask, then with distilled water diluting extremely
Graduation mark 50mL, shakes up, to be measured；Sent out using Agilent companies model 720ES full-automatic inductance coupled plasma-atomic
The weight content of metal potassium element in spectrometer analysis testing sample is penetrated, the average out to final result of three test values is taken.
4. a kind of additive for polymer as claimed in claim 1, it is characterised in that R1, R2 are expressed as ethyl, third
Base, butyl, hexyl or cyclohexyl.
5. a kind of additive for polymer as claimed in claim 1, it is characterised in that the metal potassium element, which comes from, to be contained
Potassium compound, one or more of the potassium-containing compound in potassium chloride, potassium carbonate, potassium sulfate or potassium nitrate.
6. a kind of additive for polymer as claimed in claim 1, it is characterised in that the polymer is polyester, Buddhist nun
Dragon, PPE, TPE, TPU or epoxy resin.
7. a kind of additive for polymer as claimed in claim 6, it is characterised in that the polymer is nylon 6.
8. the preparation method of a kind of additive for polymer as described in claim 1-7, it is characterised in that by dialkyl group
Hypophosphites is uniform in high-speed mixer and mixing with potassium-containing compound, obtains the additive for polymer；
Wherein, one or more of the potassium-containing compound in potassium chloride, potassium carbonate, potassium sulfate or potassium nitrate.
9. a kind of additive for polymer as described in claim 1-7 is used as the purposes of fire retardant.
10. a kind of polymeric material for including the additive for being used for polymer as described in claim 1-7, including 5-25 parts by weight
The additive for polymer, the polymer of 50-75 parts by weight or its mixture.
11. polymeric material as claimed in claim 10, it is characterised in that the polymer be polyester, nylon, PPE, TPE,
TPU or epoxy resin, preferably polyester, nylon or PPE.
12. polymeric material as claimed in claim 11, it is characterised in that the polymer is nylon 6.
13. polymeric material as claimed in claim 10, it is characterised in that filler and 0.1-5 also including 15-40 parts by weight
The auxiliary agent of parts by weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710406650.XA CN107177200A (en) | 2017-06-02 | 2017-06-02 | It is a kind of for additive of polymer and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710406650.XA CN107177200A (en) | 2017-06-02 | 2017-06-02 | It is a kind of for additive of polymer and preparation method thereof |
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| CN107177200A true CN107177200A (en) | 2017-09-19 |
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| CN201710406650.XA Pending CN107177200A (en) | 2017-06-02 | 2017-06-02 | It is a kind of for additive of polymer and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109632672A (en) * | 2019-01-09 | 2019-04-16 | 山西省化工研究所（有限公司） | A kind of quantitative detecting method of polypropylene beta crystal nucleating agent |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1280583A (en) * | 1997-11-28 | 2001-01-17 | 科莱恩有限公司 | Method for producing salts of dialkylphosphinic acids |
| US20040049063A1 (en) * | 2002-09-06 | 2004-03-11 | Clariant Gmbh | Surface-modified salts of phosphinic acid |
| CN1660857A (en) * | 2003-12-19 | 2005-08-31 | 科莱恩有限公司 | Salts of dialkylphosphinic acids |
| US7446140B2 (en) * | 2004-05-11 | 2008-11-04 | Clariant Produkte (Deutschland) Gmbh | Dialkylphosphinic salts, their use, and a process for their preparation |
| CN103788125A (en) * | 2013-12-31 | 2014-05-14 | 邓娟 | Additive for polymer and preparation method for additive |
| CN105367823A (en) * | 2015-10-30 | 2016-03-02 | 广州金凯新材料有限公司 | Additive for polymer, preparing method and application of additive, and flame-retardant polymer molding composition composed of additive |
| JP2017008211A (en) * | 2015-06-23 | 2017-01-12 | 東レ株式会社 | Polyamide resin composition and molded article thereof |
-
2017
- 2017-06-02 CN CN201710406650.XA patent/CN107177200A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1280583A (en) * | 1997-11-28 | 2001-01-17 | 科莱恩有限公司 | Method for producing salts of dialkylphosphinic acids |
| US20040049063A1 (en) * | 2002-09-06 | 2004-03-11 | Clariant Gmbh | Surface-modified salts of phosphinic acid |
| CN1660857A (en) * | 2003-12-19 | 2005-08-31 | 科莱恩有限公司 | Salts of dialkylphosphinic acids |
| US7446140B2 (en) * | 2004-05-11 | 2008-11-04 | Clariant Produkte (Deutschland) Gmbh | Dialkylphosphinic salts, their use, and a process for their preparation |
| CN103788125A (en) * | 2013-12-31 | 2014-05-14 | 邓娟 | Additive for polymer and preparation method for additive |
| JP2017008211A (en) * | 2015-06-23 | 2017-01-12 | 東レ株式会社 | Polyamide resin composition and molded article thereof |
| CN105367823A (en) * | 2015-10-30 | 2016-03-02 | 广州金凯新材料有限公司 | Additive for polymer, preparing method and application of additive, and flame-retardant polymer molding composition composed of additive |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109632672A (en) * | 2019-01-09 | 2019-04-16 | 山西省化工研究所（有限公司） | A kind of quantitative detecting method of polypropylene beta crystal nucleating agent |
| CN109632672B (en) * | 2019-01-09 | 2021-03-12 | 山西省化工研究所（有限公司） | Quantitative detection method of polypropylene beta-crystal nucleating agent |
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Application publication date: 20170919 |