CN101845153A - Inorganic powder additive-type flame retardant and preparation method thereof - Google Patents
Inorganic powder additive-type flame retardant and preparation method thereof Download PDFInfo
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- CN101845153A CN101845153A CN 201010192943 CN201010192943A CN101845153A CN 101845153 A CN101845153 A CN 101845153A CN 201010192943 CN201010192943 CN 201010192943 CN 201010192943 A CN201010192943 A CN 201010192943A CN 101845153 A CN101845153 A CN 101845153A
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Abstract
The invention provides an inorganic powder additive-type flame retardant and a preparation method thereof. The inorganic powder additive-type flame retardant comprises the following components in percentage by weight: 45 percent of SiO2, 38 percent of MgO, 2.19 percent of ZnO, 5.13 percent of Al2O3, 1.3 percent of CuO and 8.38 percent of montmorillonite. The inorganic powder additive-type flame retardant of the invention can have the effect of acid catalysis to perform a partial cross-linking reaction and carbonization on a system in a process of burning a high polymer, so a carbon coke protective layer is formed, volatile decomposers are prevented from leaking outwards and a shielding effect is achieved. Simultaneously the decomposing temperature of antimony halide oxide produced in a reaction process of a halogen flame retardant and Sb2O3 is reduced so as to assist in inflaming retarding.
Description
Technical field
The present invention relates to a kind of fire retardant, more specifically be meant a kind of inorganic powder additive-type flame retardant and preparation method thereof.
Background technology
After the 1950's, along with the macromolecular material industrial expansion, fire retardant materials such as rubber and plastic class, electrical type, building material more and more are widely used in to be produced and various fields in life.Meanwhile, since the rubber and plastic class, electrical type, and the fire that the combustibility of building material causes has also led to heavy loss of life and personal injury and has caused enormous economic loss to people.From the sixties, some industrially developed country promptly begin to produce and use fire retardant material.
Fire retardant material is a kind of protecting materials, it be can stop the burning and self and be not easy the incendiary material, solid is arranged such as materials such as cement, steel, glass; Have liquidly, also abbreviate fire retardant as, if coat fire retardant on various material surfaces such as need fire-proof wall, it can guarantee do not burnt on fire, can not make yet the combustion range aggravation, enlarge, effectively prevent the generation of fire.
With regard to output and consumption, fire retardant has become produces the indispensable material of all kinds of fire proofings at present.And fire retardant is of a great variety, and its chemical structure and using method are also had nothing in common with each other, and halogen accounts for more than 80% in the flame-retardant system of China, and inorganic system only accounts for about 17% of fire retardant, and half is wherein arranged is antimonous oxide.The in recent years continuous consumption along with new environmental requirement and new laws and regulations requirement and mineral resources reduces, and the fire retardant that the insider researchs and develops the mineral-type of new shape progressively becomes a current important topic.
Summary of the invention
The invention provides a kind of inorganic powder additive-type flame retardant, it can play the acid catalysis effect in the superpolymer combustion processes, makes partial cross-linked reaction of system and charing, thereby forms the burnt protective layer of charcoal, stops the volatility resolvent to escape, and produces shielding effect.Simultaneously also can with halogen flame and Sb
2O
3The decomposition temperature of the oxyhalogenation antimony that produces in the course of reaction reduces, thereby it is fire-retardant to reach assistance.And this is to be first purpose of the present invention.
The invention provides a kind of inorganic powder additive-type flame retardant, its bromine at plastics is in the flame-retardant system modification, can partly substitute Sb fully
2O
3Use, when reducing product cost, can also obviously improve drawing abillity, and can improve to a certain extent the Partial Physical Property intensity of modified plastics.And this is to be second purpose of the present invention.
The invention provides a kind of inorganic powder additive-type flame retardant, it has higher high whiteness, when the production white products, also can reduce the consumption of titanium dioxide, reduces production costs.And this is to be the 3rd purpose of the present invention.
A kind of preparation method of inorganic powder additive-type flame retardant, its preparation flow is simple, and preparation time is short, can prepare inorganic powder additive-type flame retardant of the present invention fast.And this is to be the 4th purpose of the present invention.
The technical solution used in the present invention is: a kind of inorganic powder additive-type flame retardant, its component comprise that weight ratio is 45% SiO
2, 38% MgO, 2.19% ZnO, 5.13% Al
2O
3, 1.3% CuO and 8.38% imvite.
A kind of preparation method of inorganic powder additive-type flame retardant, it may further comprise the steps,
The first step is 45% SiO with weight ratio
2And the MgO of weight ratio 38% puts into a container, then injects silane in this container, utilizes silane to this SiO
2And MgO carries out activation process, subsequently with this seal of vessel, makes this SiO
2And this MgO and external environment condition are isolated.
In second step, the preheating homogenizer makes the temperature of this homogenizer remain between 85 degree-95 degree,
The 3rd step, the SiO that activation process is good
2And MgO and weight ratio are 19% ZnO, 5.13% Al
2O
3, 1.3% CuO and 8.38% imvite pour into together in the homogenizers of temperature between 85 degree-95 degree and carried out high-speed stirred 10 minutes.
The 4th goes on foot, and is 45% SiO with weight ratio with four layers of paper bag
2, 38% MgO, 2.19% ZnO, 5.13% Al
2O
3, the mixture composite packaging that forms of 1.3% CuO and 8.38% imvite, to finish whole preparation process.
With this SiO
2And the time that this MgO is sealed in this container is no more than 24 hours.
Beneficial effect of the present invention has:
1. its resistance to elevated temperatures of inorganic powder additive-type flame retardant of the present invention is good, and in 400 ℃, thermal weight loss only is 0.5 ‰, the thermally-stabilised excellence of combined treatment.
2. inorganic powder additive-type flame retardant of the present invention and engineering plastic modification product as: other component in PA, PBT, PP, HIPS, PET, ABS, PVC and the PC+ABS alloy combines well, and reaching the product mechanical property can effectively be kept.
3. inorganic powder additive-type flame retardant of the present invention can cooperate with Sb2O3, reaching in the same flame retardant effect situation, can reduce by 40%～60% Sb
2O
3Consumption, play cost-effective purpose.
4. fire-retardant product can significantly improve the flowability of product adding inorganic powder additive-type flame retardant of the present invention below 3%, thereby improves the dimensional stability and the product surface smooth finish of goods.
5. fire-retardant product can significantly improve the electrical property of product after adding inorganic powder additive-type flame retardant of the present invention, comprises dielectric strength and CTI value etc.
6. can help fire-retardant product under high temperature, high humidity situation, to keep itself mechanical property and electrical property of fire-retardant product.
Embodiment
A kind of inorganic powder additive-type flame retardant, its component comprise that weight ratio is 45% SiO
2, 38% MgO, 2.19% ZnO, 5.13% Al
2O
3, 1.3% CuO and 8.38% imvite.
A kind of preparation method of inorganic powder additive-type flame retardant, it may further comprise the steps,
The first step is 45% SiO with weight ratio
2And the MgO of weight ratio 38% puts into a container, then injects silane in this container, utilizes silane to this SiO
2And MgO carries out activation process, subsequently with this seal of vessel, makes this SiO
2And this MgO and external environment condition are isolated.
It should be noted that this SiO
2And the time that this MgO is sealed in this container be no more than 24 hours, in order to avoid silane produces volatilization, affect activation effect.
In second step, the preheating homogenizer makes the temperature of this homogenizer remain between 85 degree-95 degree,
The 3rd step, the SiO that activation process is good
2And MgO and weight ratio are 19% ZnO, 5.13% Al
2O
3, 1.3% CuO and 8.38% imvite pour into together in the homogenizers of temperature between 85 degree-95 degree and carried out high-speed stirred 10 minutes.
The 4th goes on foot, and is 45% SiO with weight ratio with four layers of paper bag
2, 38% MgO, 2.19% ZnO, 5.13% Al
2O
3, the mixture composite packaging that forms of 1.3% CuO and 8.38% imvite, to finish whole preparation process.
Inorganic powder additive-type flame retardant of the present invention is a white powder, whiteness＞98%, median size 1.1um, loss on ignition＜5, have characteristics such as high whiteness, high fineness, high purity, specific surface area is big, surface effects, volume effect with ultrafine particle, no skin irritation, tasteless, non-corrosiveness.
The inorganic powder additive-type flame retardant scope of application of the present invention: be applicable to PA, PBT, PP, HIPS, PET, ABS, PVC and PC+ABS alloy plastic.
Inorganic powder additive-type flame retardant of the present invention can with halogen and usefulness, also can be used as the auxiliary of antimony, 340 ℃ of decomposition temperatures.Because this product passed through special surface treatment, greatly improved compatibility and bonding force with plastics, viscosity reducing effect is big, can increase loading, improves reinforcement; Dipping to glass fibre is good, and mixing time is short; Flow evenly forming etc. in the mould.With Sb
2O
3Compound, can significantly reduce Sb
2O
3Consumption, mechanical property conservation rate＞more than 90%.Because inorganic powder additive-type flame retardant of the present invention has higher high whiteness, when the production white products, also can reduce the consumption of titanium dioxide, reduces production costs.
Inorganic powder additive-type flame retardant of the present invention can play acid catalysis in the high polymer combustion process, make the partial cross-linked reaction of system and charing, thereby forms the burnt protective layer of charcoal, stops the volatility analyte to escape, and produces shielding action.Simultaneously also can with halogen flame and Sb
2O
3The decomposition temperature of the oxyhalogenation antimony that produces in the course of reaction reduces, and assists fire-retardant purpose thereby reach.
Its characteristics of inorganic powder additive-type flame retardant of the present invention have:
1. its resistance to elevated temperatures is good, and in 400 ℃, thermal weight loss only is 0.5 ‰, the thermally-stabilised excellence of combined treatment.
Its with the engineering plastic modification product as: other component in PA, PBT, PP, HIPS, PET, ABS, PVC and the PC+ABS alloy combines well, and reaching the product mechanical property can effectively be kept.
3. it can cooperate with Sb2O3, reaching in the same flame retardant effect situation, can reduce by 40%～60% Sb
2O
3Consumption, play cost-effective purpose.
4. fire-retardant product can significantly improve the flowability of product adding inorganic powder additive-type flame retardant of the present invention below 3%, thereby improves the dimensional stability and the product surface smooth finish of goods.
5. fire-retardant product can significantly improve the electrical property of product after adding inorganic powder additive-type flame retardant of the present invention, comprises dielectric strength and CTI value etc.
6. can help fire-retardant product under high temperature, high humidity situation, to keep itself mechanical property and electrical property of fire-retardant product.
The application of inorganic powder additive-type flame retardant of the present invention in the right system of modified plastics bromine system resistance:
The flame-retardant modified proportioning of table 1:PBT
| Sequence number | 1 | 2 | 3 | 4 | 5 |
| PBT% | 58 | 58 | 58 | 58 | 58 |
| DBDPE% | 9 | 9 | 9 | 9 | 9 |
| Sb2O3% | 3 | 2 | 1.5 | 1 | 0 |
| LHX-999% | 0 | 1.5 | 2 | 2 | 3 |
| Sequence number | 1 | 2 | 3 | 4 | 5 |
| Other | 5 | 5 | 5 | 5 | 5 |
Table 2: flame-retardant modified PBT sample detects data
| Test event | Method of testing | 1 | 2 | 3 | 4 | 5 | Unit |
| Hot strength | GB/T1040-1992 | 104 | 107 | 106 | 108 | 106 | MPa |
| Elongation at break | GB/T1040-1992 | 2.1 | 2.3 | 2.4 | 2.2 | 2.6 | % |
| Bending strength | GB/T9341-2000 | 137 | 136 | 139 | 140 | 139 | MPa |
| Bending modulus | GB/T9341-2000 | 7981 | 8106 | 7930 | 8008 | 8219 | MPa |
| Notched Izod impact strength | GB/T1843-1996 | 8.2 | 8.4 | 8.5 | 8.4 | 8.6 | KJ/m2 |
| Heat distortion temperature | GB/T1634-2004 | 219 | 221 | 220 | 218 | 219 | ℃ |
| Melt index | GB/T3682-2000 | 27.3 | 31 | 32.5 | 34.1 | 37 | G/10mi n |
| Anti-flammability | UL-94 | V-0 | V-0 | V-0 | V-1 | HB | / |
| Ash | GB/T9345-1988 | 24.3 | 25.1 | 25.5 | 24.8 | 25.3 | % |
The flame-retardant modified proportioning of table 3:PA
| Sequence number | 6 | 7 | 8 | 9 | 10 |
| PA66% | 56 | 56 | 56 | 56 | 56 |
| DBDPE% | 10 | 10 | 10 | 10 | 10 |
| Sb2O3% | 4 | 3 | 2 | 1.5 | 0 |
| LHX-999% | 0 | 1 | 2 | 2.5 | 4 |
| Other | 5 | 5 | 5 | 5 | 5 |
| GF% | 25 | 25 | 25 | 25 | 25 |
Table 4: flame-retardant modified PA sample detects data
| Test event | Method of testing | 6 | 7 | 8 | 9 | 10 | Unit |
| Hot strength | GB/T1040-1992 | 144 | 150 | 149 | 153 | 155 | MPa |
| Elongation at break | GB/T1040-1992 | 2.8 | 2.6 | 2.9 | 3.1 | 3.0 | % |
| Bending strength | GB/T9341-2000 | 183 | 195 | 191 | 197 | 196 | MPa |
| Bending modulus | GB/T9341-2000 | 7670 | 7809 | 7783 | 7841 | 7952 | MPa |
| Notched Izod impact strength | GB/T1843-1996 | 15.3 | 16.1 | 16.2 | 16.7 | 17.1 | KJ/m2 |
| Test event | Method of testing | 6 | 7 | 8 | 9 | 10 | Unit |
| Heat distortion temperature | GB/T1634-2004 | 253 | 255 | 254 | 255 | 253 | ℃ |
| Melt index | GB/T3682-2000 | / | / | / | / | / | G/10mi n |
| Anti-flammability | UL-94 | V-0 | V-0 | V-0 | V-1 | HB | / |
| Ash | GB/T9345-1988 | 25.6 | 24.8 | 25.3 | 24.9 | 25.5 | % |
According to the proportioning of table 1 with table 3, the detection data of difference associative list 2 and table 4, can find, after in the flame-retardant modified system of PBT, PA, adding inorganic powder additive-type flame retardant of the present invention respectively, its results change is similar substantially, the most tangible to be exactly melt flow rate (MFR) improve with the increase of the addition of inorganic powder additive-type flame retardant of the present invention, and other mechanical properties remain unchanged substantially, help the forming process of material like this.Replacing the Sb of half in addition
2O
3The time, all can keep original flame retardant effect, but be still can not substitute Sb fully in the flame-retardant system at bromine
2O
3Because inorganic powder additive-type flame retardant of the present invention belongs to inorganic particle, compare Sb
2O
3More can guarantee the environmental requirement of material; Most importantly the price of inorganic powder additive-type flame retardant of the present invention only is equivalent to Sb
2O
3/ 3rd of a market price, and its source of goods is not subjected to the restriction of metallic mineral resources, can greatly reduce the cost of flame-retardant modified PBT, PA, is conducive to the market competition of fire proofing.In addition, in the flame-retardant modified system of PA, add inorganic powder additive-type flame retardant of the present invention after, the color of product obviously bleaches, and more helps the outward appearance of product and painted.
The flame-retardant modified proportioning of table 5:ABS
| Sequence number | 11 | 12 | 13 | 14 | 15 |
| ABS% | 81 | 81 | 81 | 81 | 81 |
| DBDPE% | 12 | 12 | 12 | 12 | 12 |
| Sb2O3% | 4 | 2.5 | 2 | 1.5 | 0 |
| LHX-999% | 0 | 1.5 | 2 | 2.5 | 4 |
| Other | 3 | 3 | 3 | 3 | 3 |
Table 6: flame-retardant modified ABS sample detects data
| Test event | Method of testing | 11 | 12 | 13 | 14 | 15 | Unit |
| Hot strength | GB/T1040-1992 | 39.3 | 41.0 | 40.7 | 40.8 | 41.5 | MPa |
| Elongation at break | GB/T1040-1992 | 18.6 | 21.3 | 20.3 | 23.8 | 21.6 | % |
| Bending strength | GB/T9341-2000 | 58 | 57 | 60 | 58 | 61 | MPa |
| Bending modulus | GB/T9341-2000 | 2491 | 2511 | 2485 | 2527 | 2508 | MPa |
| Notched Izod impact strength | GB/T1843-1996 | 12.1 | 12.4 | 12.2 | 12.6 | 13.2 | KJ/m2 |
| Melt index | GB/T3682- | 3.1 | 4.2 | 4.8 | 5.9 | 6.5 | G/10mi |
| 2000 | n | ||||||
| Anti-flammability | UL-94 | V-0 | V-0 | V-0 | V-1 | HB | / |
| Density | GB/T1033-1986 | 1.20 | 1.18 | 1.16 | 1.15 | 1.13 | G/cm3 |
According to the proportioning of table 5, the detection data of associative list 6 find out, in the flame-retardant modified system of ABS, add inorganic powder additive-type flame retardant of the present invention after, except melt flow rate (MFR) improves with the increase of its addition, along with Sb
2O
3Progressively replaced, the impact strength of material slightly improves, and proportion then obviously descends; Be when replacing half or with interior Sb in the flame-retardant system at bromine
2O
3The time, can keep original flame retardant effect equally.In addition, use inorganic powder additive-type flame retardant of the present invention to replace Sb
2O
3After, the flame-retardant modified product appearance color of extruding bleached than in the past, and the tinting strength, tinting power of product is also stronger.
The flame-retardant modified proportioning of PP
| Sequence number | 16 | 17 | 18 | 19 | 20 |
| PP% | 60 | 60 | 60 | 60 | 60 |
| DBDPE% | 18 | 18 | 18 | 18 | 18 |
| Sb2O3% | 6 | 4 | 3 | 2.5 | 0 |
| LHX-999% | 0 | 2 | 3 | 3.5 | 6 |
| Other | 16 | 16 | 16 | 16 | 16 |
Table 8: flame-retardant modified PP sample detects data
| Test event | Method of testing | 16 | 17 | 18 | 19 | 20 | Unit |
| Hot strength | GB/T1040-1992 | 24.3 | 23.7 | 25.5 | 25.3 | 24.2 | MPa |
| Elongation at break | GB/T1040-1992 | 32 | 36 | 35 | 41 | 38 | % |
| Bending strength | GB/T9341-2000 | 36 | 38 | 36 | 35 | 37 | MPa |
| Bending modulus | GB/T9341-2000 | 2209 | 2187 | 2241 | 2133 | 2270 | MPa |
| Notched Izod impact strength | GB/T1843-1996 | 3.6 | 3.9 | 3.8 | 4.2 | 4.2 | KJ/m2 |
| Melt index | GB/T3682-2000 | 9.4 | 11.1 | 11.9 | 13.4 | 15.7 | G/10mi n |
| Test event | Method of testing | 16 | 17 | 18 | 19 | 20 | Unit |
| Heat distortion temperature | GB/T1634-2004 | 130 | 132 | 132 | 133 | 134 | ℃ |
| Anti-flammability | UL-94 | V-0 | V-0 | V-1 | V-1 | HB | / |
| Density | GB/T1033-1986 | 1.23 | 1.20 | 1.19 | 1.17 | 1.14 | G/cm3 |
According to the proportioning of table 7 and the detection data of table 8, we are very easy to find, and are behind the adding inorganic powder additive-type flame retardant of the present invention, the same with flame-retardant modified ABS in the flame-retardant modified system of PP, along with Sb
2O
3Progressively replaced, the melt flow rate (MFR) of material, impact strength all improve with the increase of the addition of inorganic powder additive-type flame retardant of the present invention, and proportion then obviously descends; Be when replacing 1/3rd or with interior Sb in the flame-retardant system at bromine
2O
3The time, also can keep original flame retardant effect.Equally, using inorganic powder additive-type flame retardant of the present invention to replace Sb
2O
3After, the flame-retardant modified product appearance color of extruding bleached than in the past, and surface gloss and tinting strength, tinting power also all have some improvement.In addition, because inorganic powder additive-type flame retardant of the present invention is a ultrafine inorganic powder, in flame-retardant modified PP product, add inorganic powder additive-type flame retardant of the present invention, can play certain nucleogenesis, can shorten the shaping cycle of material, the heat-drawn wire of material also slightly improves, and can suitably reduce the consumption of special-purpose nucleator in the modifying process, plays the purpose that further reduces cost.
The flame-retardant modified proportioning of table 9:HIPS
| Sequence number | 21 | 22 | 23 | 24 | 25 |
| HIPS% | 79 | 79 | 79 | 79 | 79 |
| DBDPE% | 13 | 13 | 13 | 13 | 13 |
| Sb2O3% | 4.5 | 2.5 | 2 | 1.5 | 0 |
| LHX-999% | 0 | 2 | 2.5 | 3 | 4.5 |
Table 10: flame-retardant modified HIPS sample detects data
| Test event | Method of testing | 21 | 22 | 23 | 24 | 25 | Unit |
| Hot strength | GB/T1040-1992 | 24.3 | 25.1 | 24.8 | 25.1 | 25.3 | MPa |
| Elongation at break | GB/T1040-1992 | 49 | 61 | 52 | 60 | 69 | % |
| Bending strength | GB/T9341-2000 | 43 | 45 | 43 | 47 | 44 | MPa |
| Bending modulus | GB/T9341-2000 | 2180 | 2231 | 2209 | 2287 | 2313 | MPa |
| Notched Izod impact strength | GB/T1843-1996 | 11.8 | 12.3 | 12.4 | 12.7 | 12.6 | KJ/m2 |
| Melt index | GB/T3682-2000 | 8.8 | 9.3 | 9.4 | 9.7 | 9.6 | G/10mi n |
| Anti-flammability | UL-94 | V-0 | V-0 | V-1 | HB | HB | / |
| Density | GB/T1033-1986 | 1.15 | 1.13 | 1.12 | 1.10 | 1.09 | G/cm3 |
Proportioning according to table 9, the detection data of associative list 10, can find that behind the adding inorganic powder additive-type flame retardant of the present invention, its result is basic identical with the effect that adds inorganic powder additive-type flame retardant of the present invention in the flame-retardant modified system of ABS in the flame-retardant modified system of HIPS.
Inorganic powder additive-type flame retardant of the present invention is in the flame-retardant system modification at the bromine of plastics, can partly substitute Sb fully
2O
3Use, when reducing product cost, can also obviously improve drawing abillity, and can improve to a certain extent the Partial Physical Property intensity of modified plastics.
Claims (3)
1. inorganic powder additive-type flame retardant, it is characterized in that: its component comprises that weight ratio is 45% SiO
2, 38% MgO, 2.19% ZnO, 5.13% Al
2O
3, 1.3% CuO and 8.38% imvite.
2. the preparation method of an inorganic powder additive-type flame retardant is characterized in that, it may further comprise the steps,
The first step is 45% SiO with weight ratio
2And the MgO of weight ratio 38% puts into a container, then injects silane in this container, utilizes silane to this SiO
2And MgO carries out activation process, subsequently with this seal of vessel, makes this SiO
2And this MgO and external environment condition are isolated;
In second step, the preheating homogenizer makes the temperature of this homogenizer remain between 85 degree-95 degree;
The 3rd step, the SiO that activation process is good
2And MgO and weight ratio are 19% ZnO, 5.13% Al
2O
3, 1.3% CuO and 8.38% imvite pour into together in the homogenizers of temperature between 85 degree-95 degree and carried out high-speed stirred 10 minutes;
The 4th goes on foot, and is 45% SiO with weight ratio with four layers of paper bag
2, 38% MgO, 2.19% ZnO, 5.13% Al
2O
3, the mixture composite packaging that forms of 1.3% CuO and 8.38% imvite, to finish whole preparation process.
3. the preparation method of a kind of inorganic powder additive-type flame retardant as claimed in claim 2 is characterized in that, with this SiO
2And the time that this MgO is sealed in this container is no more than 24 hours.
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| CN110128818A (en) * | 2019-05-28 | 2019-08-16 | 武汉顺威赛特工程塑料有限公司 | A kind of low cost high-glowing-filament-temperature flame-retardancy nylon material and its preparation method and application |
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