CN106674594A - Intercalated layered double hydroxide smoke inhibitor and preparation method thereof - Google Patents

Intercalated layered double hydroxide smoke inhibitor and preparation method thereof Download PDF

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Publication number
CN106674594A
CN106674594A CN201611089694.6A CN201611089694A CN106674594A CN 106674594 A CN106674594 A CN 106674594A CN 201611089694 A CN201611089694 A CN 201611089694A CN 106674594 A CN106674594 A CN 106674594A
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smoke
smoke suppressant
preparation
double hydroxide
layered double
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林彦军
李凯涛
段雪
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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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
    • C08K7/00—Use of ingredients characterised by shape
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
    • C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
    • C01F7/785—Hydrotalcite
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM

Abstract

The invention discloses an intercalated layered double hydroxide smoke inhibitor and a preparation method thereof. The smoke inhibitor is a layered structural material formed by assembling a laminated sheet consisting of metal cations and interlayer anions, wherein a specific composition general formula of the smoke inhibitor is M<2+>1-xM<3+>x(OH)2(A<n->)n/2.mH2O. According to the preparation method disclosed by the invention, the intercalated layered double hydroxide smoke inhibitor is prepared by adopting a one-step coprecipitation method or a clean hydrothermal reaction at one step; the preparation method is simple and practical; according to the obtained intercalated layered double hydroxide smoke inhibitor, smoke inhibiting groups such as molybdate anions, an octamolybdate radical, a cuprate radical and a stannate radical are arranged at an interlayer, and smoke inhibiting elements such as iron and copper are introduced into the laminated sheet, so that a good carbon forming effect is realized, the smoke generating amount can be reduced, and the smoke inhibiting effect is synergically enhanced; meanwhile, a layered double hydroxide laminated sheet forms an alkaline porous substance at high temperature; the alkaline porous substance has greater specific surface area and can effectively adsorb smog; the prepared intercalated layered double hydroxide smoke inhibitor is applied to an ordinary rubber-plastic product and a high-temperature rubber-plastic product; the maximum density (Ds, max) at low additive amount (1phr) can be reduced by 87.3 percent; the intercalated layered double hydroxide smoke inhibitor is remarkable in smoke inhibiting effect and is a smoke inhibitor material with excellent performance.

Description

A kind of intercalated houghite smoke suppressant and preparation method thereof
Technical field：
The invention belongs to press down cigarette technical field of material, more particularly to a kind of intercalated houghite smoke suppressant and its preparation side Method, the smoke suppressant material can significantly reduce smoke density when product of rubber and plastic burns.
Background technology：
Product of rubber and plastic is played an important role in people live, every aspect of its product application in people live, For the mankind production, life provide important leverage.Product of rubber and plastic has excellent performance, but most products are readily burned, There is the significant damage that the life given people during fire incident and property safety are brought.Pass through in major part product of rubber and plastic at present Fire retardant is added to improve fire resistance, but most fire retardant smoke suppressings are poor or even part fire retardant can reduce smoke-suppressing Energy.And according to incompletely statistics, in the death by accident of fire, 80% is because the asphyxia that cigarette and toxic gas are caused causes. Therefore, the generation for reducing smog and pernicious gas when Rubber-plastic product is burnt is particularly significant to protection personal safety, exploitation New suppression cigarette material is significant.
Layered double hydroxide (Layered Double Hydroxides, abbreviation LDHs), also known as hydrotalcite, be One class novel lamellar functional material.Due to unique supramolecular structure, its main layer board composition, interlayer guest molecule species and number Amount etc. has Modulatory character, and is widely used in the fields such as catalysis, electricity, optics.Inventor grinds in European patent 02100800 A kind of LDHs fire proofings are studied carefully, LDHs has abundant CO due to interlayer3 2-With structure H2O, the anti-flammability gas CO when being heated2 And H2O releases play a part of starvation and reduce material surface temperature, while it can form condensed phase on surface, prevent combustion Burning face extends, and with good fire retardation, but smoke suppressing is general.
The content of the invention：
To improve the smoke suppressing of product of rubber and plastic, further development presses down cigarette material, the invention provides a kind of intercalation neatly Stone smoke suppressant and preparation method thereof.Such intercalated houghite not only maintains the flame retarding and smoke suppressing properties of hydrotalcite itself, and utilizes Interlayer suppression cigarette group such as molybdate, eight molybdates, copper acid group, stannate radicle and the copper that can be introduced into main layer board, iron etc. press down Cigarette element have it is good acted on into charcoal, collaboration plays the smoke suppressing that suppression cigarette effect effectively improves such material.
Described intercalated houghite smoke suppressant is that the laminate being made up of metal cation assembles layered with interlayer anion Structural material, its concrete composition formula is M2+ 1-xM3+ x(OH)2(An-)n/2·mH2O, wherein M2+Represent divalent metal Mg2 +、Zn2+、Ni2+、Co2+、Fe2+、Cu2+In one or two, it is preferred that Mg2+、Zn2+In one or two；M3+Represent three Valency metal cation Al3+、Ni3+、Co3+、Fe3+In one kind, it is preferred that Al3+；Interlayer anion An-It is molybdate, eight molybdic acids One kind in root, copper acid group or stannate radicle, n is anion valence number；X is M3+Molar fraction, its span is 0.2≤ x≤0.4；M represents the quantity of the crystallization water, 0≤m≤6.
The preparation method one of described intercalated houghite smoke suppressant：By soluble divalent metal salt and soluble trivalent metal Salt is in molar ratio M2+/M3+The ratio of=1-10 is made into mixing salt solution in being dissolved in deionized water, wherein [M2+]=0.1- 2mol/L；One or more mixed ammonium/alkali solutions with NaOH in molybdate, octamolybdate, cuprate or stannate are prepared, its The molal quantity and M of middle NaOH2+And M3+The ratio of molal quantity sum is 1.5-2.5, the molybdate of addition, octamolybdate, cuprate Or the total moles and M of one or more in stannate3+Mol ratio is 1-5；The volume of the mixing aqueous slkali of preparation is mixing 0.5-2 times of salting liquid volume；By fast nucleation in mixing salt solution and mixing aqueous slkali simultaneously addition rotating liquid-film reactor, Under nitrogen protection, 80-140 DEG C of crystallization 0.1-72h obtains intercalated houghite smoke suppressant to the slurries for obtaining after washing, drying.
The preparation method two of described intercalated houghite smoke suppressant：By M2+Hydroxide and M3+Hydroxide according to M2 +/M3+Mol ratio is mixed for the ratio of 1-4, according to interlayer anion An-/M3+Mol ratio is the ratio of 1-5 by H2MoO4、 MoO3Or stannic acid is added in said mixture, the deionized water of 0.25-999 times of solid gross mass is added；It is pre- by grinding Treatment, is then transferred in high pressure crystallizing kettle, at 100-300 DEG C, opens stirring, and setting speed of agitator is 50-500rpm, reaction Solid product is taken out after 0.1-3 days, is dried after directly filtering, obtain intercalated houghite smoke suppressant.
Above-mentioned intercalated houghite smoke suppressant as the smoke suppressant of product of rubber and plastic application.
Described product of rubber and plastic include rubber, PVC, EVA, PE, PP, PS, PC, PA, PA66, PET, PBT, PS, PVA, ABS。
The addition of the intercalated houghite smoke suppressant is 1-100wt%, more preferably preferably 1-98wt%, 1-10wt%.
Beneficial outcomes：The present invention is made intercalated houghite suppression cigarette using a step coprecipitation or the cleaning step of hydro-thermal reaction one Agent, the preparation method is simple and practical, the intercalated houghite smoke suppressant for obtaining due to interlayer have suppression cigarette group such as molybdenum acid ion, The suppression cigarette element such as eight molybdates, copper acid group and stannate radicle and the iron, the copper that are introduced into laminate have it is good acted on into charcoal, can subtract Smoke, cooperative reinforcing smoke suppressing effect are given birth to less, while neatly stone veneer forms Alkaline porous material at high temperature, with larger ratio Surface greatly can effective adsorbing smoke.Obtained intercalated houghite smoke suppressant is applied to common product of rubber and plastic and high temperature rubber and plastic system In product, (1phr) maximum smoke density D under few additives,max87.3% can be reduced, smoke suppressing effect is a class excellent performance significantly Smoke suppressant material.
Brief description of the drawings：
Fig. 1 is the XRD spectra of molybdate intercalated houghite prepared by embodiment 1；
Fig. 2 is the smoke density test chart of molybdate intercalated houghite/EVA composites prepared by embodiment 1；
Fig. 3 is stannate radicle intercalated houghite SEM spectrograms prepared by embodiment 2.
Specific embodiment：
For a better understanding of the present invention, it is with reference to the embodiment content that the present invention is furture elucidated but of the invention Content is not limited solely to the following examples.
Embodiment 1：
Step：It is 30kg by gross mass, mol ratio is 2:1:3 Mg (OH)2、Al(OH)3And H2MoO4It is added separately to In 60kg deionized waters, pre-processed by grinder, be made Mg (OH)2、Al(OH)3And H2MoO4Slurries, take the 10kg slurries and add Enter in autoclave；215 DEG C of reaction temperature is warming up to, 6h is reacted under stirring condition (350rpm), the product for obtaining is in 70 DEG C drying 8 hours, obtains molecular formula for Mg4Al2(OH)12MoO4·4H2The molybdate intercalated houghite smoke suppressant of O.
Crystal Structure is carried out to product using the XRD-6000 type X-ray powder diffraction instrument of Japanese Shimadzu Corporation, is schemed 1 is XRD spectra.It can be seen that occurring in that Mg at 2 θ=11.58 °, 23.47 °, 34.87 ° and 60.8 ° or so places2Al- MoO4The characteristic diffraction peak of-LDHs, and peak shape point is towering, baseline is low flat, illustrates product crystal structural integrity, and crystalline phase is single.
Take in 1g molybdate intercalated houghite smoke suppressant addition 100g EVA obtained above, distinguish in two-roll mill It is well mixed in 150 DEG C of mill 40min, by the mixing material after refining on compression molding instrument in 150 DEG C, 100 kilograms of pressure Under be pressed into 1mm prints for smoke density test.It is not added with the EVA prints D of layered double hydroxide smoke suppressants,max(most Big smoke density) it is 239.15, add the EVA prints D of molybdate intercalated houghite smoke suppressants,maxIt is 30.25, have dropped 87.35%, specific maximum smoke density test chart is shown in Fig. 2.Molybdate intercalated houghite smoke suppressant effectively increases composite Smoke suppressing.
The maximum smoke density test data of the different suppression cigarette materials of table 1 and EVA composites
As can be seen from Table 1, non-intercalated houghite has certain smoke suppressing effect under 10phr additions, and most opium is close Degree have dropped 43.51%, and molybdate intercalated houghite shows excellent smoke suppressing under the addition of 1phr, maximum Smoke density have dropped 87.35%, and its smoke suppressing is significantly excellent in non-intercalated houghite, while its addition is low (1phr), It is smaller to its mechanical property and other performance impacts in product of rubber and plastic use, it is easy to use.
Embodiment 2：
By Mg (NO3)2、Zn(NO3)2With Al (NO3)3By Mg/Zn/Al=3:1:2 ratio is made into mixing salt solution, makes [Mg2+]=1.2mol/L, by NaOH and Na2SnO3By n (Na2SnO3)/n(Al3+)=2, n (NaOH)/[n (Mg2+)+n(Zn2+)+ n(Al3+)]=1.5 ratio is made into mixed ammonium/alkali solutions, mixing salt solution is identical with mixed ammonium/alkali solutions volume, and two kinds of solution are same When add rotating liquid-film reactor, the slurries for obtaining are heated with stirring to 80 DEG C under nitrogen environmental protection in flask, react 24h Stannate radicle intercalated houghite smoke suppressant is obtained by washing.
Using the supra55 type scanning electron microscopic observation crystallite dimensions and pattern of German ZEISS companies.Fig. 3 is SEM photograph, As seen from the figure, obtained product structure composition is uniform, uniform particle diameter.
Take in 3g stannate radicle intercalated houghite smoke suppressant addition 100g PVC obtained above, distinguish in two-roll mill It is well mixed in 140 DEG C of mill 50min, by the mixing material after refining on compression molding instrument in 145 DEG C, 100 kilograms of pressure Under be pressed into 1.5mm prints for smoke density test.It is not added with the PVC prints D of layered double hydroxide smoke suppressants,max (maximum smoke density) is 450, adds the PVC prints D of stannate radicle intercalated houghite smoke suppressants,maxIt is 143, have dropped 68.2%, Stannate radicle intercalated houghite smoke suppressant effectively increases the smoke suppressing of PVC composites.

Claims (6)

1. a kind of intercalated houghite smoke suppressant, it is characterised in that the intercalated houghite smoke suppressant is made up of metal cation Laminate and interlayer anion be assembled into layer structure material, its concrete composition formula is M2+ 1-xM3+ x(OH)2(An-)n/2· mH2O, wherein M2+Represent divalent metal Mg2+、Zn2+、Ni2+、Co2+、Fe2+、Cu2+In one or two, it is preferred that Mg2+、Zn2+In one or two；M3+Represent trivalent metal cation Al3+、Ni3+、Co3+、Fe3+In one kind, it is preferred that Al3+；Interlayer anion An-It is molybdate, the one kind in eight molybdates, copper acid group or stannate radicle, n is anion valence number；x It is M3+Molar fraction, its span is 0.2≤x≤0.4；M represents the quantity of the crystallization water, 0≤m≤6.
2. the preparation method of intercalated houghite smoke suppressant according to claim 1, it is characterised in that its concrete operations condition For：It is in molar ratio M by soluble divalent metal salt and soluble trivalent metal salt2+/M3+The ratio of=1-10 is dissolved in deionization Mixing salt solution is made into water, wherein [M2+]=0.1-2mol/L；In preparation molybdate, octamolybdate, cuprate or stannate One or more mixed ammonium/alkali solutions with NaOH, the wherein molal quantity and M of NaOH2+And M3+The ratio of molal quantity sum is 1.5-2.5, the total moles of one or more and M in the molybdate of addition, octamolybdate, cuprate or stannate3+Mole Than being 1-5；The volume of the mixing aqueous slkali of preparation is 0.5-2 times of mixing salt solution volume；By mixing salt solution and mixing alkali Solution simultaneously add rotating liquid-film reactor in fast nucleation, the slurries for obtaining under nitrogen protection, 80-140 DEG C of crystallization 0.1- 72h, intercalated houghite smoke suppressant is obtained after washing, drying.
3. the preparation method of intercalated houghite smoke suppressant according to claim 1, it is characterised in that its concrete operations condition For：By M2+Hydroxide and M3+Hydroxide according to M2+/M3+Mol ratio is mixed for the ratio of 1-4, cloudy according to interlayer Ion An-/M3+Mol ratio is the ratio of 1-5 by H2MoO4、MoO3Or stannic acid is added in said mixture, solid is added total The deionized water of 0.25-999 times of quality；Pre-processed by grinding, be then transferred in high pressure crystallizing kettle, at 100-300 DEG C, opened Stirring, setting speed of agitator is 50-500rpm, and reaction takes out solid product after 0.1-3 days, is dried after directly filtering, and is inserted Layer hydrotalcite smoke suppressant.
4. intercalated houghite smoke suppressant according to claim 1 as the smoke suppressant of product of rubber and plastic application.
5. application according to claim 4, it is characterised in that described product of rubber and plastic include rubber, PVC, EVA, PE, PP、PS、PC、PA、PA66、PET、PBT、PS、PVA、ABS。
6. application according to claim 4, it is characterised in that intercalated houghite smoke suppressant the adding in product of rubber and plastic Dosage is 1-100wt%, preferably 1-98wt%, more preferably 1-10wt%.
CN201611089694.6A 2016-11-30 2016-11-30 Intercalated layered double hydroxide smoke inhibitor and preparation method thereof Pending CN106674594A (en)

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CN107523375A (en) * 2017-08-22 2017-12-29 成都新柯力化工科技有限公司 A kind of lubricating oil special antiwear agent and preparation method thereof
CN107774283A (en) * 2017-10-24 2018-03-09 中南大学 A kind of molybdenum disulfide hybrid hydrotalcite composite material and its preparation method and application
CN107793671A (en) * 2017-11-03 2018-03-13 常州市万昌化工有限公司 A kind of preparation method of heat conductive flame-retarding soft PVC
CN108636400A (en) * 2018-04-28 2018-10-12 东北师范大学 A kind of hydrotalcite composite catalyst and its preparation method and application
CN108659514A (en) * 2018-06-02 2018-10-16 北京化工大学 A kind of preparation and application of the efficient smoke suppressant of polyurethane
CN109824974A (en) * 2018-12-24 2019-05-31 万华化学（宁波）有限公司 A kind of halogen-free flame-retardant composite material and preparation method thereof of high flowing antibacterial
CN109928427A (en) * 2019-03-21 2019-06-25 暨南大学 A kind of double ion intercalation molybdenum oxide nanometer sheet, hetero-junctions and preparation method thereof
CN110194872A (en) * 2019-05-09 2019-09-03 北京化工大学 A kind of PVC smoke suppressant and preparation method thereof
CN113104871A (en) * 2021-04-25 2021-07-13 北京化工大学 Method for preparing magnesium-aluminum hydrotalcite from magnesite

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CN107523375B (en) * 2017-08-22 2020-01-31 辽宁汽众润滑油生产有限公司 antiwear agent special for lubricating oil and preparation method thereof
CN107523375A (en) * 2017-08-22 2017-12-29 成都新柯力化工科技有限公司 A kind of lubricating oil special antiwear agent and preparation method thereof
CN107774283A (en) * 2017-10-24 2018-03-09 中南大学 A kind of molybdenum disulfide hybrid hydrotalcite composite material and its preparation method and application
CN107774283B (en) * 2017-10-24 2020-02-14 中南大学 Molybdenum disulfide intercalated hydrotalcite composite material and preparation method and application thereof
CN107793671A (en) * 2017-11-03 2018-03-13 常州市万昌化工有限公司 A kind of preparation method of heat conductive flame-retarding soft PVC
CN108636400A (en) * 2018-04-28 2018-10-12 东北师范大学 A kind of hydrotalcite composite catalyst and its preparation method and application
CN108636400B (en) * 2018-04-28 2021-01-15 东北师范大学 Hydrotalcite-based composite catalyst and preparation method and application thereof
CN108659514A (en) * 2018-06-02 2018-10-16 北京化工大学 A kind of preparation and application of the efficient smoke suppressant of polyurethane
CN108659514B (en) * 2018-06-02 2020-11-03 北京化工大学 Preparation and application of polyurethane efficient smoke suppressant
CN109824974A (en) * 2018-12-24 2019-05-31 万华化学（宁波）有限公司 A kind of halogen-free flame-retardant composite material and preparation method thereof of high flowing antibacterial
CN109928427A (en) * 2019-03-21 2019-06-25 暨南大学 A kind of double ion intercalation molybdenum oxide nanometer sheet, hetero-junctions and preparation method thereof
CN110194872A (en) * 2019-05-09 2019-09-03 北京化工大学 A kind of PVC smoke suppressant and preparation method thereof
CN113104871A (en) * 2021-04-25 2021-07-13 北京化工大学 Method for preparing magnesium-aluminum hydrotalcite from magnesite
CN113104871B (en) * 2021-04-25 2022-07-26 北京化工大学 Method for preparing magnalium hydrotalcite from magnesite

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