CN107163287A - 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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- CN107163287A CN107163287A CN201710382367.8A CN201710382367A CN107163287A CN 107163287 A CN107163287 A CN 107163287A CN 201710382367 A CN201710382367 A CN 201710382367A CN 107163287 A CN107163287 A CN 107163287A
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
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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
- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
-
- 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
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2268—Ferrous oxide (FeO)
-
- 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
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2272—Ferric oxide (Fe2O3)
-
- 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
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
-
- 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
- C08K2003/3072—Iron sulfates
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 ferro element, wherein weight content of the metal ferro element in total additive are 10 480ppm.Additive preparation technology of the invention containing particular range content metal ferro element is simple, production cost is low, it is applied in polymer, and the absolute value of the front and rear inherent viscosity difference of polymer composition injection can be made to be less than 0.15dl/g, and the polymer composition has 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 ferro 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 ferro element in fire retardant dialkylphosphinic salts,
The higher fire resistance of polymer composition can not only be ensured, inherent viscosity is poor before and after can also making polymer composition injection
The absolute value of value is less than 0.15dl/g.
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 ferro element is added in salt, obtained polymer composition can be made to possess excellent fire resistance, meanwhile, polymer
The absolute value of inherent viscosity difference is less than 0.15dl/g before and after composition injection.
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 ferro element, wherein weight content of the metal ferro element in total additive are 10-480ppm.Preferred weight
Content is 30-350ppm, and more preferably weight content is 50-200ppm, and further preferred weight content is 70-150ppm.
The method of testing of the weight content of metal ferro 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 ferro 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 ferro element comes from iron content simple substance or iron containing compoundses, and iron containing compoundses are selected from di-iron trioxide, four
Fe 3 O, ferrous oxide, ferrous sulfate, ferric sulfate, ammonium ferric sulfate, iron ammonium sulfate, ferrous nitrate, ferric nitrate, protochloride
One or more in iron, iron chloride.The source of metal ferro element pointed by the present invention is not limited only to the example above, no matter makes
With the iron containing compoundses of which kind of form, atomic emission spectrometry can be used to detect.The weight content of metal ferro element is
By metal ferro element in itself rather than on the basis of adding the iron containing compoundses of metal ferro element.The metallic iron 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 is obtained by the way that dialkyl hypophosphorous acid salt and iron content simple substance or iron containing compoundses is uniform in high-speed mixer and mixing
To the additive for polymer；
Wherein, iron containing compoundses are selected from di-iron trioxide, ferroso-ferric oxide, ferrous oxide, ferrous sulfate, ferric sulfate, sulphur
One or more in sour iron ammonium, iron ammonium sulfate, ferrous nitrate, ferric nitrate, frerrous chloride, iron chloride.
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 ferro 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 absolute value of the front and rear inherent viscosity difference of polymer composition injection can also be made to be less than 0.15dl/g.
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 iron content：Do not detect；
PA6：PA6M2000 (Meida Nylon Co., Ltd., Xinhui, Guangdong)
Glass fibre：ECS301-HP (Chongqing Polycomp International Co., Ltd)；
Antioxidant：1010, (Jin Haiyabao)；
Iron containing compoundses used of the invention are purchased in market.
The method of testing of the weight content of metal ferro 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 ferro 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 method of testing of inherent viscosity of the present invention：In concentrated sulfuric acid, obtained by following formula at 30 DEG C, 0.05g/dl,
Logarithmic viscosity number (the η of the sample of 0.1g/dl, 0.2g/dl, 0.4g/dl concentrationinh), concentration 0 will be extended down to outside it, by income value
It is used as inherent viscosity [η].Wherein, t0Represent solvent Drain time (second), t1The Drain time (second) of sample solution is represented, C is represented
The concentration (g/dl) of sample in solution.When sample solution contains solid matter, by filter of the solid matter with 0.5 μm of aperture
Filtering, gained filtrate is used to determine.
ηinh=[ln (t1/t0)]/C
The absolute value of inherent viscosity difference before and after polymer composition injection of the present invention：Use day smart Resin Industry strain
80 tons of injection (mo(u)lding) machines of formula commercial firm manufacture, are detained 10 minutes at 300 DEG C of barrel temperature, and then injection of polymer composition is simultaneously
The inherent viscosity before injecting and after injection is determined, the absolute value of the inherent viscosity difference before and after injection is smaller more excellent.
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 iron containing compoundses 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 iron content chemical combination in preparation process for the additive metal iron content 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 polymer composition under foregoing test condition
The absolute value of inherent viscosity difference before and after injection, 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 ferro element, wherein weight content of the metal ferro element in total additive are 10-480ppm.
2. a kind of additive for polymer as claimed in claim 1, it is characterised in that the metal ferro element adds always
Plus the weight content in agent is 30-350ppm, preferred weight content is 50-200ppm, and more preferably weight content is 70-
150ppm。
3. a kind of additive for polymer as claimed in claim 1 or 2, it is characterised in that the weight of metal ferro 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 ferro 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 ferro element comes from
Iron content simple substance or iron containing compoundses, iron containing compoundses are selected from di-iron trioxide, ferroso-ferric oxide, ferrous oxide, ferrous sulfate, sulphur
One or more in sour iron, ammonium ferric sulfate, iron ammonium sulfate, ferrous nitrate, ferric nitrate, frerrous chloride, iron chloride.
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 iron containing compoundses, obtains the additive for polymer；
Wherein, the metal ferro element comes from iron content simple substance or iron containing compoundses, and iron containing compoundses are selected from di-iron trioxide, four
Fe 3 O, ferrous oxide, ferrous sulfate, ferric sulfate, ammonium ferric sulfate, iron ammonium sulfate, ferrous nitrate, ferric nitrate, protochloride
One or more in iron, iron chloride.
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.
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| CN201710382367.8A CN107163287A (en) | 2017-05-26 | 2017-05-26 | It is a kind of for additive of polymer and preparation method thereof |
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| CN201710382367.8A CN107163287A (en) | 2017-05-26 | 2017-05-26 | It is a kind of for additive of polymer and preparation method thereof |
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Citations (3)
| 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 |
| CN103102367A (en) * | 2013-02-27 | 2013-05-15 | 广州金凯新材料有限公司 | Preparation method and application of dialkyl phosphinate with high density and large diameter |
| 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 |
-
2017
- 2017-05-26 CN CN201710382367.8A patent/CN107163287A/en active Pending
Patent Citations (3)
| 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 |
| CN103102367A (en) * | 2013-02-27 | 2013-05-15 | 广州金凯新材料有限公司 | Preparation method and application of dialkyl phosphinate with high density and large diameter |
| 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 |
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