CN109111654A - A kind of PVC smoke suppressant and preparation method thereof - Google Patents
A kind of PVC smoke suppressant and preparation method thereof Download PDFInfo
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- CN109111654A CN109111654A CN201810823126.7A CN201810823126A CN109111654A CN 109111654 A CN109111654 A CN 109111654A CN 201810823126 A CN201810823126 A CN 201810823126A CN 109111654 A CN109111654 A CN 109111654A
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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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
- C08K3/28—Nitrogen-containing compounds
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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
- C08K3/32—Phosphorus-containing compounds
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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
- C08K3/38—Boron-containing compounds
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-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
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
Abstract
The invention discloses a kind of PVC smoke suppressants and preparation method thereof.The smoke suppressant is that a kind of ZnO of modification coats hydrotalcite, is expressed as ZnO/LDHs.The present invention uses the method for generating ZnO in the surface in situ of hydrotalcite that ZnO is coated to hydrotalcite surface, so that ZnO is tightly combined with hydrotalcite, and ZnO has biggish specific surface area, the catalysis carbon-forming effect of ZnO and the physical barrier effect of hydrotalcite occur on molecular level when therefore as smoke suppressant, with stronger synergy, the inhibitory effect to flue gas is greatly improved.Therefore ZnO cladding hydrotalcite is a kind of outstanding smoke suppressant.The smoke amount for adding PVC after such smoke suppressant is reduced up to 70%.
Description
Technical field:
The invention belongs to plastic additive technical fields, and in particular to a kind of ZnO cladding hydrotalcite PVC smoke suppressant of modification
And preparation method thereof.
Technical background:
2016, the whole nation was informed of a case fire 31.2 ten thousand altogether, died 1582 people, hurt 1065 people, and 37.2 hundred million yuan of direct property loss.
Flue gas harm to the human body is very big, has data to show, when fire due to anoxic, flue gas infringement caused by casualties it is dead up to fire
Die 50-the 80% of number.Smoke particle in flue gas has complete bridging effect to visible light, when flue gas diffuses, it is seen that light by
The masking of smoke particle and weaken significantly, visibility substantially reduces, and flue gas has great stimulation to the eyes of people, and making one cannot
It opens eyes, people just affects travel speed in evacuation.The phobic fear caused on human psychological of flue gas.Especially occur
When flashing over, flame and flue gas go out door and window hole, and raging fire is raging, Dark smoke billows, makes one to generate very big fear, when will cause evacuation
Confusion.
Polyvinyl chloride (PVC) is with its excellent electrical property, chemical corrosion resistance, anti-flammability, stability and cheap valence
Lattice and to be widely used in agricultural, construction industry, wire and cable industry, communication, health care, interior decoration, automobile, aircraft etc. numerous
Industry and field.But the life smoke of PVC is big, ranks first in common plastics, thus inhibits particularly significant to the flue gas of PVC.
The smoke yields for reducing PVC facilitate the escape of personnel in fire, reduce casualties and economic loss.
CN201510998943 discloses hydrotalcite-like material and has obvious effects on for flame retardant of plastic and suppression cigarette, text
It offers: hydrotalcite/zinc class compound composite modified polyvinyl chloride combustion characteristics, Su Hu, Zhejiang University, 2011-06:6-7, report
Nano hydrotalcite can make smoke density reduce by 59.2% after participating in PVC in-situ polymerization, but in-situ polymerization technique is more complex, practical
Using constant, and hydrotalcite decreases to the reduction amplitude effect of PVC smoke density in common blending processing.Document PVC/
The research of nano hydrotalcite composite material smoke-suppressing, Zheng Xiuting, Wu great Ming, Liu Ying, Zhu Fuhua, Chinese Plastics, 2003 (8): 36-39
Hydrotalcite is had studied for the suppression cigarette of hard PVC, when adding hydrotalcite 5%, the smoke density range of decrease about 30%.Document: hydrotalcite pair
The fire-retardant influence with hot property of soft pvc, Qu Hongqiang, Wu Weihong, Li Yunpeng, Yuan Huijie, Xu Jianzhong, functional material increase 38:
2807-2809 has studied different types of hydrotalcite to the fire-retardant and smoke suppressing effect of flexible PVC, when adding 20%, smoke density
The maximum range of decrease is about 28%.ZnO has the function of being catalyzed PVC into charcoal, can assist to reduce smoke density, document nanometer in burning
Hydrotalcite/influence of the zinc oxide smoke-inhibiting flame retardant compound system to flexible PVC performance, plastics 2007 (6): adds in PVC in 8-11
Add 5 parts of LDHs/ZnO Complex Smokes, smoke density grade is reduced to 70.1 from 95.8.
The present invention has coated ZnO on the surface of hydrotalcite, so that the physical barrier of the catalysis carbon-forming effect and hydrotalcite of ZnO
It acts on and generates synergy on molecular level, compared with the PVC for not adding smoke suppressant, the range of decrease of smoke density is up to 70%；Packet
Hydrotalcite after covering ZnO has carried out surface organic modification, enhances its dispersibility in resin.
Summary of the invention
The object of the present invention is to provide a kind of smoke suppressants and preparation method thereof for reducing PVC smoke density.
Smoke suppressant provided by the present invention is ZnO cladding hydrotalcite, is expressed as ZnO/LDHs, wherein the chemical formula of LDHs
Are as follows:The value range of x is 2-3 in formula；An-Represent anion One of；N is the charge number of anion.
Smoke suppressant provided by the present invention the preparation method is as follows:
A. prepared by hydrotalcite:
It is that 2-3 weighs Mg (OH) by Mg:Al molar ratio2With Al (OH)3, water is added to be configured to the slurry that solid content is 1-15%
Liquid is warming up to 120-250 DEG C, and addition contains An-Acid or be passed through CO2Gas is stirred to react 2-24h, obtains hydrotalcite slurry.
Described contains An-Acid be: H2CO3、H3PO4、HNO3And H3BO3, sour additional amount meets above-mentioned LDHs chemical formula
It is required that；
B oxide coated by zinc:
Zinc salt is added in the hydrotalcite slurry of step A, the additional amount of zinc salt is the 0.2-10% of hydrotalcite quality, is added
Heat arrives 60-150 degree, adds lye, and the additional amount of lye is according to react generation Zn (OH) with zinc salt2To calculate；React 0.5-
For 24 hours, by slurry wash 1-5 times after reaction, the hydrotalcite slurry of coating zinc oxide is obtained, adding water to be made into solid content is 0.5-
25% slurries are stand-by；
The zinc salt be one or more of zinc sulfate, zinc chloride, zinc nitrate,
The lye is the aqueous solution of one or both of sodium hydroxide, potassium hydroxide, concentration 1-25%.
The surface of C coating zinc oxide hydrotalcite is modified:
The hydrotalcite slurry of step B is warming up to 60-100 DEG C, modifying agent is added, amount of modifier is slurry solid content
1-10% stirs lower reaction 0.5-24h；Filtering, by filter cake in 130-200 DEG C of dry 2-24h to get to modification ZnO/LDHs.
The modifying agent is the fatty acid or fatty acid salt silane coupling agent, titanate coupling agent, Aluminate of C12-18
One or more of coupling agent.
The ZnO/LDHs of above-mentioned preparation is used to do smoke suppressant in PVC, application effect test is carried out, the results are shown in Table 2, by table
2 visible smoke suppressants can make the reduction amplitude of smoke density reach 70%.
Beneficial effects of the present invention:
1, ZnO carries out in-situ preparation on the surface of hydrotalcite, and the specific surface area of hydrotalcite is larger, so that ZnO is with larger
Specific surface area, more resin matrixes can be contacted, it is more efficient.
2, ZnO is generated in the surface in situ of hydrotalcite, and ZnO is tightly combined with hydrotalcite, the catalysis carbon-forming effect of ZnO and water
The physical barrier effect of talcum occurs on molecular level, has stronger synergy.
3, the organically-modified dispersibility for enhancing ZnO/LDHs smoke suppressant in PVC on surface.
Specific embodiment:
Embodiment 1
Hydrotalcite preparation:
Weigh 58g Mg (OH)2With 39g Al (OH)3, add water to be configured to the slurries that solid content is 10%, be warming up to 150 DEG C,
It is passed through CO2, it is stirred to react 6h, obtains the slurries of hydrotalcite, wherein solid content is 16.3%.
Oxide coated by zinc:
Slurries 307g is weighed, wherein hydrotalcite levels 50g is made, white vitriol 3.55g is weighed and is added to above-mentioned neatly
In stone slurries, 60 DEG C are heated to, then 0.99g sodium hydroxide is configured to 10% aqueous solution, is added drop-wise in hydrotalcite slurry, is dripped
The reaction was continued 4h after complete, is filtered, washed 2 times, and the filter cake after washing is configured to the slurries that solid content is 0.5-25% again.
The surface of coating zinc oxide hydrotalcite is modified:
The hydrotalcite slurry of above-mentioned coating zinc oxide is warming up to 80 DEG C, modifying agent stearic acid is added, amount of modifier is
The 4% of slurry solid content stirs lower reaction 1h；Filtering, by 150 DEG C of filter cake dry 6h, obtains ZnO/LDHs smoke suppressant, wherein
ZnO content is the 2% of LDHs, and the chemical formula of hydrotalcite LDHs is Mg2Al(OH)6(CO3)0.5·2H2O。
PVC smoke suppressant is added in PVC according to 3 kinds of formulas in table 1 and is mixed, at 180 DEG C of melting temperature, molding temperature
The sheet material test smoke density of 1mm is kneaded, is processed at 180 DEG C of degree.Formula 1 is soft goods formula, and formula 2 is boardy product formula,
Formula 3 is transparent article formula.Smoke density test is according to GB/T8323.2-2008.Smoke density test result is shown in Table 2.
1 PVC difference article formulations of table
Embodiment 2
Hydrotalcite preparation:
Weigh Mg (OH)287g, Al (OH)339g.By Mg (OH)2With Al (OH)3The slurries for becoming solid content 5% are prepared,
85% phosphoric acid 57.6g is added and is warming up to 160 DEG C, is stirred to react 8h, obtains the slurries of hydrotalcite, solid content 8.5%.
Oxide coated by zinc:
Slurries 588g is weighed, its solid content 50g is made, zinc chloride 3.36g is weighed and is added in above-mentioned hydrotalcite slurry, add
Heat is configured to 30% aqueous solution to 80 degree, then by 1.98g sodium hydroxide；It is added drop-wise in hydrotalcite slurry, the reaction was continued after dripping off
6h washs modified hydrotalcite 3 times, and the filter cake after washing is configured to the slurries that solid content is 0.5-25%.
The surface of coating zinc oxide hydrotalcite is modified:
The hydrotalcite slurry of above-mentioned coating zinc oxide is warming up to 80 DEG C, modifying agent calcium stearate, amount of modifier is added
It is the 4% of slurry solid content, stirs lower reaction 2h.Slurries are filtered, filter cake is obtained, 150 DEG C of filter cake dry 6h can be obtained
PVC smoke suppressant 2, wherein ZnO content is the 4% of LDHs, the chemical formula of hydrotalcite are as follows:
Mg3Al(OH)8(PO3)0.33·2H2O。
Smoke density test is carried out with embodiment 1, the results are shown in Table 2.
Embodiment 3
Hydrotalcite preparation:
Weigh Mg (OH)269.6g, Al (OH)339g, preparing becomes the slurries that solid content is 15%, and boric acid is added
185.5g is warming up to 170 DEG C, is stirred to react 10h, obtains the slurries of hydrotalcite, solid content 24.1%.
Oxide coated by zinc:
Slurries 207g is weighed, its solid content 50g is made, zinc nitrate hexahydrate 9.18g is weighed and is added in hydrotalcite slurry
90 degree are heated to, then 2.48g sodium hydroxide is configured to 40% aqueous solution, is added drop-wise in hydrotalcite slurry, is continued after dripping off anti-
3h is answered, modified hydrotalcite is washed 4 times, the filter cake after washing is configured to the stone slurries of solid content 0.5-25%.
The surface of coating zinc oxide hydrotalcite is modified:
The hydrotalcite slurry of above-mentioned coating zinc oxide is warming up to 80 DEG C, modifying agent zinc laurate, amount of modifier is added
It is the 4% of slurry solid content, stirs lower reaction 2h, 180 DEG C of filter cake dry 6h is obtained ZnO/LDHs smoke suppressant, wherein ZnO by filtering
Content is the 5% of LDHs, and the chemical formula of hydrotalcite is Mg2.4Al(OH)6.8H2BO3·2H2O。
Smoke density test is carried out with embodiment 1, the results are shown in Table 2.
Embodiment 4
Hydrotalcite preparation:
Weigh Mg (OH)263.8g, Al (OH)339g, preparing becomes the slurries that solid content is 5%, is added 65%
H3NO350g is warming up to 170 DEG C, is stirred to react 10h, obtains the slurries of hydrotalcite, solid content 10.1%.
Oxide coated by zinc:
Slurries 495g is weighed, its solid content 50g is made, zinc chloride 8.40g is weighed and is added in above-mentioned hydrotalcite slurry, add
Heat is configured to 20% aqueous solution to 80 degree, then by 6.92gKOH；It is added drop-wise in hydrotalcite slurry, the reaction was continued 6h after dripping off will
Modified hydrotalcite washs 5 times, and the filter cake after washing is configured to the slurries that solid content is 0.5-25%.
The surface of coating zinc oxide hydrotalcite is modified:
The hydrotalcite slurry of above-mentioned coating zinc oxide is warming up to 80 DEG C, modifying agent Silane coupling reagent KH-570 is added, changes
Property agent dosage be the 3% of slurry solid content, stir and lower react 2h.Slurries are filtered, filter cake is obtained, by 190 DEG C of dryings of filter cake
12h can obtain ZnO/LDHs smoke suppressant, and wherein ZnO content is the 10% of LDHs, and the chemical formula of hydrotalcite is Mg2.2Al(OH)6.4NO3·2H2O。
Smoke density test is carried out with embodiment 1, the results are shown in Table 2.
Comparative example 1:
Using currently used smoke suppressant -- industrial hydrotalcite DHT-4A carries out suppression cigarette as a comparison case, with above-described embodiment
Contrast on effect, the chemical formula of DHT-4A are Mg4.3Al2(OH)12.6(CO3)·4H2O.Smoke density survey is carried out as described in Example 1
Examination, the results are shown in Table 2.
Table 2
| Maximum smoke density | Formula 1 | Formula 2 | Formula 3 |
| Embodiment 1 | 156 | 137 | 183 |
| Embodiment 2 | 224 | 182 | 212 |
| Embodiment 3 | 213 | 213 | 176 |
| Embodiment 4 | 229 | 193 | 209 |
| Comparative example 1 | 316 | 294 | 389 |
| Without smoke suppressant | 505 | 476 | 565 |
From 2 result of table as it can be seen that PVC smoke suppressant prepared by the present invention is suitable for soft goods, boardy product and transparent PVC formula
In, smoke suppressing effect is clearly, more excellent using hydrotalcite smoke suppressing effect than merely, because of the Louis that Zn is generated in combustion
This acid ZnCI2The de- HCI of PVC can be promoted to react, form trans- polyene structure, reduce intramolecular cyclization and generate benzene and its spread out
A possibility that biological.It is less to add the PVC of the smoke suppressant flue gas that generates when fire occurs, when leaving people for and more escaping
Between, the loss of life and property can be reduced.Simple addition hydrotalcite reduces amplitude substantially in 30- as smoke suppressant smoke density
40%, and this smoke suppressant can make the reduction amplitude of smoke density reach 70%.
Claims (2)
1. a kind of PVC smoke suppressant, which is ZnO cladding hydrotalcite, is expressed as ZnO/LDHs, wherein the chemical formula of LDHs
Are as follows:X=2-3 in formula；An-Represent anionIn
It is a kind of；N is the charge number of anion.
2. a kind of method for preparing PVC smoke suppressant described in claim 1, the specific steps are as follows:
A. prepared by hydrotalcite:
It is that 2-3 weighs Mg (OH) by Mg:Al molar ratio2With Al (OH)3, add water to be configured to the slurries that solid content is 1-15%, rise
For temperature to 120-250 DEG C, addition contains An-Acid or be passed through CO2Gas is stirred to react 2-24h, obtains hydrotalcite slurry；
Described contains An-Acid be: H2CO3、H3PO4、HNO3And H3BO3, sour additional amount meets above-mentioned LDHs chemical formula and wants
It asks；
B. oxide coated by zinc:
Zinc salt is added in the hydrotalcite slurry of step A, the additional amount of zinc salt is the 0.2-10% of hydrotalcite quality, is heated to
60-150 degree, adds lye, and the additional amount of lye generates Zn (OH) according to reacting with zinc salt2To calculate；0.5-24h is reacted,
By slurry wash 1-5 times after reaction, the hydrotalcite slurry of coating zinc oxide is obtained, water is added to be made into solid content as 0.5-25% slurry
Liquid is stand-by；
The zinc salt be one or more of zinc sulfate, zinc chloride, zinc nitrate,
The lye is the aqueous solution of one or both of sodium hydroxide, potassium hydroxide, concentration 1-25%；
C. the surface of coating zinc oxide hydrotalcite is modified:
The hydrotalcite slurry of step B is warming up to 60-100 DEG C, modifying agent is added, amount of modifier is the 1- of slurry solid content
10%, stir lower reaction 0.5-24h；Filtering, by filter cake in 130-200 DEG C of dry 2-24h to get to ZnO/LDHs；
The modifying agent is coupled for the fatty acid or fatty acid salt silane coupling agent, titanate coupling agent, Aluminate of C12-18
One or more of agent.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111607124A (en) * | 2020-05-21 | 2020-09-01 | 科迈特新材料有限公司 | Calcium-doped zinc-aluminum hydrotalcite-nano zinc oxide composite material and preparation method thereof |
| CN112573568A (en) * | 2019-09-27 | 2021-03-30 | 中国石油化工股份有限公司 | L-acid-rich hydrotalcite and preparation method and application thereof |
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| JP2003064234A (en) * | 2001-06-12 | 2003-03-05 | Hosei:Kk | Resin composition with low harmful chlorine content for gasket |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112573568A (en) * | 2019-09-27 | 2021-03-30 | 中国石油化工股份有限公司 | L-acid-rich hydrotalcite and preparation method and application thereof |
| CN112573568B (en) * | 2019-09-27 | 2023-04-07 | 中国石油化工股份有限公司 | L-acid-rich hydrotalcite and preparation method and application thereof |
| CN111607124A (en) * | 2020-05-21 | 2020-09-01 | 科迈特新材料有限公司 | Calcium-doped zinc-aluminum hydrotalcite-nano zinc oxide composite material and preparation method thereof |
| CN111607124B (en) * | 2020-05-21 | 2022-05-27 | 科迈特新材料有限公司 | Calcium-doped zinc-aluminum hydrotalcite-nano zinc oxide composite material and preparation method thereof |
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