CN103382676A - Flame retardant paper containing rare earth-containing hydrotalcite, and preparation method and application thereof - Google Patents
Flame retardant paper containing rare earth-containing hydrotalcite, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses flame retardant paper containing rare earth-containing hydrotalcite, and a preparation method and an application thereof. The preparation method of the flame retardant paper containing the rare earth-containing hydrotalcite comprises the steps: firstly, synthesizing binary, ternary, quaternary, pentabasic or hexabasic hydrotalcite containing lanthanum, cerium, samarium, terbium, europium and other rare earth elements, then directly adding 5 to 300 parts of the rare earth-containing hydrotalcite into 100 parts of paper fibers by an intra-pulp addition method, a dipping method or a coating method, or modifying 100 parts of the paper fibers with 5 to 300 parts of the rare earth-containing hydrotalcite by a self-assembly method, and finally papermaking in a paper former to obtain the flame retardant paper. The flame retardant paper containing the rare earth-containing hydrotalcite utilizes the synergistic flame retardant function of the rare earth elements, so the flame retardant effect is substantially improved, and the mechanical properties are excellent. The flame retardant paper containing the rare earth-containing hydrotalcite has the characteristics of environmental protection, high efficiency and no pollution; the preparation method of the flame retardant paper is simple and diverse, and is suitable for industrial production. The flame retardant paper containing the rare earth-containing hydrotalcite can be widely applied to packaging, building and living paper and other fields.
Description
Technical field
The present invention relates to material science, particularly a kind of rare earth hydrotalcite fire retardant papers and its preparation method and application that contains.
Background technology
Paper material take string as raw material is extensive with its raw material sources, and printing performance is good, is convenient to Compound Machining, be convenient to suitability for industrialized production, be convenient to transportation, cost is low, lightweight, the advantages such as discarded object recoverable and degradable are widely used in the fields such as packing, building, decoration.But paper material is easy to burning, and burning velocity is exceedingly fast, and their contact fire will turn to dust and ashes, and their materials that ignites of fire normally, or promotes the intensity of a fire and rapidly develop, and many fire are that paper material is caused by igniting.The disaster hidden-trouble that is brought by paper material has become the social concern of global concern, changes its inflammability and also more and more is subject to people's great attention.From the angle of security against fire, paper material all must be through flame treatment in particular for the paper material of the aspects such as packing, building.Paper material is carried out flame treatment can reduce disaster hidden-trouble, stop and delay propagation of flame trend, win the time of putting out a fire to save life and property, reduce fire damage.Therefore, it is also very necessary the paper bag material being carried out flame treatment.At present, mainly by adding fire retardant, wherein most widely used is halogen containing flame-retardant to the fire retardant papers that China produces.But, discharging a large amount of smog and poisonous, harmful corrosive gas during general Halogen fire proofing breaking out of fire, the personnel's cause of death in fire incident is relevant with dense smoke and the toxic gas of material production more than 80%.Therefore, research and development Halogen, fire proofing tool efficient, nontoxic, environmental protection are of great significance.
Layered di-hydroxyl composite metal oxidate (Layered Double Hydroxides, be called for short LDHs) be hydrotalcite (Hydrotalcite, be called for short HT) and houghite compound (Hydrotalcite-Like Compounds, abbreviation HTLCs) general designation, a series of supramolecular materials of being assembled by these compound intercalations are called hydrotalcite intercalation material (being called for short LDHs).Its chemical composition general formula is: [M
2+ 1-xM
3+ x(OH)
2]
z+[A
n-]
z/nMH
2O。LDHs is when being heated, and its constitution water and laminate hydroxyl and interlayer anion are with water and CO
2Form deviate from, play and reduce burning gases concentration, intercept O
2The fire retardation of gas; And can reduce harmful effect to the base material physical property, the oxygen index (OI) when being conducive to improve burning is strengthened flame retardant effect; LDHs forms porous, composite metal oxide that specific surface is large after 500 ℃ of-600 ℃ of pyrolytics, the smog that produces in the absorption combustion process, thus play the cigarette effect that presses down.The constitution water of LDHs, laminate hydroxyl and interlayer anion break away from laminate in the different temperatures scope, thereby can (200 ~ 800 ℃) discharge fire-retardant species in a big way; In fire-retardant process, caloric receptivity is large, the high temperature that produces when being conducive to reduce burning.The significant flame retardant effect of LDHs and special physicochemical property can be realized few addition and high flame retarding efficiency, thereby reach real highly effective flame-retardant.At present, LDHs is mainly used in catalysis, absorption, ion-exchange, and the research in flame retardant area is relatively less, and some researcher has synthesized binary LDHs (as MgAl-CO
3) and ternary LDHs (as MgAlZn-CO
3), and be applied in flame retarded polymeric material.At present, the domestic research and comparison that LDHs is applied in fire retardant papers is few.Patent " a kind of preparation method of LDHs fire retardant papers " is by adding MgAlZnFe-CO
3The fire retardant papers of hydrotalcite preparation has certain flame retardant effect, but the improvement of its flame retardant effect is limited.
Rare earth is widely used in polymeric material field, has unique effect about research has shown rare earth compound improving macromolecular material processing and the application performance such as plastics, rubber, fiber, coating and give the aspect such as the new function of macromolecular material; As: lanthanide series compound can be used as the heat stabilizer of PVC.Compare with traditional fire retardant such as antimonous oxide, the rare earth flame resistance agent has potential Halogen, efficient, low cigarette, the characteristics such as multi-functional, and lanthana has been applied in the expansion type flame retardant system as fire retarding synergist, to improve the flame retardant effect of fire proofing.As seen, rare earth has potential using value aspect fire-retardant.
At present, domestic also have much rare earth oxide and hydrotalcite are used as fire retardant, but be all generally as flame retardant, also need another main flame retardant.So just make technique more complicated, increased production cost.In addition, most of research report is all to contain the application of rare earth element LDHs in flame-proofed polymer material, and the application study in fire retardant papers has no bibliographical information.
In order to improve the flame retardant effect of LDHs in fire retardant papers, this patent is introduced the rare earth element preparation and is contained the rare earth element hydrotalcite on the laminate of LDHs, then adopt distinct methods to add in the paper fiber containing the rare earth hydrotalcite, or the paper fiber is carried out modification, the preparation fire retardant papers.This type of contains the synergistic fire retardation that rare earth hydrotalcite fire retardant papers is utilized rare earth element, and its flame retardant effect is significantly improved, and good mechanical performance.In addition, this patent invention what contain that rare earth hydrotalcite fire retardant papers adopts is a kind of halogen-free flame retardants, have environmental protection, efficient, free of contamination characteristics; This fire retardant papers preparation method is simple, various, is suitable for industrial production.This rare earth hydrotalcite fire retardant papers that contains can be widely used in the fields such as packing, building and paper for daily use.
Summary of the invention
The purpose of this invention is to provide a kind of rare earth hydrotalcite fire retardant papers that contains.
Another object of the present invention is to provide the above-mentioned preparation method who contains rare earth hydrotalcite fire retardant papers.
The object of the present invention is achieved like this: at first synthetic binary, ternary, quaternary, five yuan or the hexa-atomic hydrotalcite that contains the rare earth elements such as lanthanum, cerium, samarium, terbium, europium, then 5 ~ 300 parts of hydrotalcites are directly added in 100 parts of paper fibers or by self-assembly method 100 parts of paper fibers are carried out modification by starching interior additive process, infusion process, rubbing method, copy paper at last on paper industry former, prepare fire retardant papers.Utilized the synergistic fire retardation of rare earth element, made paper have excellent flame retardant effect.
Concrete technical scheme of the present invention is as follows:
Under room temperature, salting liquid A and aqueous slkali B are added in the self-control reactor, the pH value of conditioned reaction liquid makes it remain at 9～10.After the question response drop is complete, being stirred a period of time in reactor after, the reactant liquor that obtains moves in there-necked flask 90 ℃ of lower crystallization 6 h, then centrifugation, obtaining the LDHs filter cake with deionized water washing, is then the 1%-10%(mass fraction with the deionized water configuration concentration) LDHs colloidal solution.Getting a certain amount of absolute dried paper pulp discongests with deionized water in the standard fibre dissociation device and is made into suspension, then can directly adopt additive process in traditional slurry, infusion process and rubbing method will be above synthetic contain rare earth LDHs colloidal solution and paper pulp mixes, or which floor employing molecular deposition, self-assembly method coat with the paper fiber surface and contain rare earth LDHs; To contain the good paper fiber of rare earth LDHs modification copies in quick sheet former and gets the preparation fire retardant papers again.Made fire retardant papers is quantitatively 120 g/m
2
The rear earth containing hydrotalcite that uses in the present invention has following chemical formula: [M
2+ 1-x-yM
3+ xRe
3+ y(OH)
- 2] [A
n-]
X+y/nMH
2O, wherein Re is rare earth element.Form the common bivalent metal ion of LDHs Mg is arranged
2+, Zn
2+, Ni
2+, Co
2+, Cu
2+, Ca
2+, Mn
2+Trivalent metal ion has A1
3+, Cr
3+, Co
3+, Fe
3+, Sc
3+, V
3+Trivalent rare earth CATION Re
3+Can be Eu
3+, Tb
3+, Sm
3+, Tm
3+, Ho
3+, Er
3+, Nd
3+, Pm
3+, Yb
3+, Lu
3+, Sc
3+, r
3+, La
3+, Ce
3+, Pr
3+, Gd
3+Or Dy
3+The content of hydrotalcite rare earth elements (Re) should satisfy 0＜Re
3+/ [Re
3++ M
3+]≤0.5(mol ratio).The mol ratio that trivalent metal compound in the raw materials of hydrotalcite accounts for total metallic compound should satisfy 0.2≤(M
3++ Re
3+)/(M
2++ M
3++ Re
3+)≤0.3.
The hydrotalcite that the present invention adds can be organically-modified hydrotalcite, the modifier that uses can be odium stearate, dodecyl sodium sulfate, sodium hydrogen tartrate, itaconic acid, glycerin monostearate, silane coupler and polyethylene glycol, its consumption is 5 ~ 50 parts (quality), and method of modifying can be coprecipitation, ion-exchange or roasting restoring method.
Compared with prior art, the present invention has the following advantages:
(1) this patent invention what contain that rare earth hydrotalcite fire retardant papers adopts is a kind of halogen-free flame retardants, have environmental protection, free of contamination characteristics.
(2) fire retardant papers of the present invention's preparation, technique is simple, various, and cost is low, is suitable for industrial production.
(3) this patent invention contains the rare earth hydrotalcite and can in the situation that do not add flame retardant and use separately, have significant flame retardant effect.
The specific embodiment
The below provides example so that the present invention will be described in more detail; it is important to point out that following examples can not be interpreted as the restriction to the invention protection domain; the person skilled in the art in this field to some nonessential improvement and adjustment that the present invention makes, must belong to protection scope of the present invention according to the foregoing invention content.
Embodiment 1
Get 0.9 mol MgCl
26H
2O, 0.3 mol AlCl
36H
2O, 0.3 mol ZnCl
2, 0.1 mol FeCl
36H
2O is dissolved in wiring solution-forming A in deionized water; With 2.56 mol NaOH, 0.8 mol Na
2CO
3Wiring solution-forming B.Under room temperature, solution A, solution B are added in the self-control reactor, the pH value of conditioned reaction liquid makes it remain at 9～10.After the question response drop is complete, being stirred a period of time in reactor after, the reactant liquor that obtains moves in there-necked flask, 90 ℃ of lower crystallization 6 h, then centrifugation, obtaining quaternary MgAlZnFe-LDHs filter cake with deionized water washing, is then the 4%(mass fraction with the deionized water configuration concentration) LDHs colloidal solution.
Get a certain amount of absolute dried paper pulp and discongest the suspension that is made into 2 % in the standard fibre dissociation device, utilize the interior additive process of slurry that above synthetic MgAlZnFe-LDHs colloidal solution and paper pulp are mixed, wherein the addition of LDHs is 100% (mass fraction) of oven dry stock, copies in quick sheet former and gets fire retardant papers.
Embodiment 2
Get 0.9 mol MgCl
26H
2O, 0.3 mol AlCl
36H
2O, 0.36 mol ZnCl
2, 0.04 mol LaCl
36H
2O is dissolved in wiring solution-forming A in deionized water; With 2.56 mol NaOH, 0.8 mol Na
2CO
3Wiring solution-forming B.Under room temperature, solution A, solution B are added in the self-control reactor, the pH value of conditioned reaction liquid makes it remain at 9～10.After the question response drop is complete, being stirred a period of time in reactor after, the reactant liquor that obtains moves in there-necked flask, 90 ℃ of lower crystallization 6 h, then centrifugation, obtaining quaternary MgAlZnLa-LDHs filter cake with deionized water washing, is then the 4%(mass fraction with the deionized water configuration concentration) LDHs colloidal solution.
Get a certain amount of absolute dried paper pulp and discongest the suspension that is made into 2 % in the standard fibre dissociation device, utilize the interior additive process of slurry that above synthetic MgAlZnLa-LDHs colloidal solution and paper pulp are mixed, wherein the addition of LDHs is 100% (mass fraction) of oven dry stock, copies in quick sheet former and gets fire retardant papers.
Embodiment 3
Get 0.9 mol MgCl
26H
2O, 0.3 mol AlCl
36H
2O, 0.38mol ZnCl
2, 0.02 mol CeCl
36H
2O is dissolved in wiring solution-forming A in deionized water; With 2.56 mol NaOH, 0.8 mol Na
2CO
3Wiring solution-forming B.Under room temperature, solution A, solution B are added in the self-control reactor, the pH value of conditioned reaction liquid makes it remain at 9～10.After the question response drop is complete, being stirred a period of time in reactor after, the reactant liquor that obtains moves in there-necked flask, 90 ℃ of lower crystallization 6 h, then centrifugation, obtaining quaternary MgAlZnCe-LDHs filter cake with deionized water washing, is then the 4%(mass fraction with the deionized water configuration concentration) LDHs colloidal solution.
Get a certain amount of absolute dried paper pulp and discongest the suspension that is made into 2 % in the standard fibre dissociation device, utilize the interior additive process of slurry that above synthetic MgAlZnCe-LDHs colloidal solution and paper pulp are mixed, wherein the addition of LDHs is 100% (mass fraction) of oven dry stock, copies in quick sheet former and gets fire retardant papers.
Embodiment 4
Get 0.9 mol MgCl
26H
2O, 0.3 mol AlCl
36H
2O, 0.38 mol ZnCl
2, 0.02 mol CeCl
36H
2O is dissolved in wiring solution-forming A in deionized water; With 2.56 mol NaOH, 0.8 mol Na
2CO
3Wiring solution-forming B.Under room temperature, solution A, solution B are added in the self-control reactor, the pH value of conditioned reaction liquid makes it remain at 9～10.After the question response drop is complete, being stirred a period of time in reactor after, the reactant liquor that obtains moves in there-necked flask, 90 ℃ of lower crystallization 6 h, then centrifugation, obtaining quaternary MgAlZnCe-LDHs filter cake with deionized water washing, is then the 1%-10%(mass fraction with the deionized water configuration concentration) LDHs colloidal solution.
Get a certain amount of absolute dried paper pulp and discongest the suspension that is made into 2 % in the standard fibre dissociation device, utilize the interior additive process of slurry that above synthetic MgAlZnCe-LDHs colloidal solution and paper pulp are mixed, wherein the addition of LDHs is 200% (mass fraction) of oven dry stock, copies in quick sheet former and gets fire retardant papers.
Embodiment 5
Get 0.9 mol MgCl
26H
2O, 0.3 mol AlCl
36H
2O, 0.38 mol ZnCl
2, 0.02 mol LaCl
36H
2O is dissolved in wiring solution-forming A in deionized water; With 2.56 mol NaOH, 0.8 mol Na
2CO
3Wiring solution-forming B.Under room temperature, solution A, solution B are added in the self-control reactor, the pH value of conditioned reaction liquid makes it remain at 9～10.After the question response drop is complete, being stirred a period of time in reactor after, the reactant liquor that obtains moves in there-necked flask, 90 ℃ of lower crystallization 6 h, then centrifugation, obtaining quaternary MgAlZnLa-LDHs filter cake with deionized water washing, is then the 4%(mass fraction with the deionized water configuration concentration) LDHs colloidal solution.
Get a certain amount of absolute dried paper pulp and discongest the suspension that is made into 2 % in the standard fibre dissociation device, it is 4% LDH colloidal solution (wherein the addition of LDHs is 100% mass fraction of oven dry stock) that paper pulp fiber after being filtered dry is immersed concentration, is filtered dry with the ultra-pure water washing after stirring certain hour.Afterwards it is immersed certain density APAM solution, be filtered dry with the ultra-pure water washing after 5min.Repeat twice above-mentioned steps and will prepare 2 layers of LDH/APAM film at pulp fiber surface.Each post-depositional paper pulp fiber all uses the ultra-pure water washing and carefully is filtered dry, and copies in quick sheet former at last and gets fire retardant papers.
After pressing GB/T14656-2009 processing fire retardant papers, adopt the SH5304 type testing vertical flammability machine of Guangzhou letter standing grain Electronics Equipment Co., Ltd to carry out the vertical combustion performance test to the fire retardant papers of embodiment 1-6 preparation; Test data is as shown in table 1 below:
Table 1 contains the fire resistance of variety classes LDHs paper
| ? | The method of inspection | Technical indicator | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| The LDHs type | ? | ? | MgAlZnFe-LDHs | MgAlZnLa-LDHs | MgAlZnCe-LDHs | MgAlZnCe-LDHs | MgAlZnLa-LDHs |
| The preparation method | ? | ? | Interior additive process | Interior additive process | Interior additive process | Interior additive process | Molecular deposition |
| LDHs addition (with respect to the absolute dried paper pulp mass fraction) | ? | ? | 100% | 100% | 100% | 200% | 200% |
| Re 3+/[Re 3++ M 3+] | ? | ? | 0 | 1/10 | 1/20 | 1/20 | 1/20 |
| Afterflame time (s) | GB/T14656-2009 | ≤5 | 3.12 | 1.83 | 1.58 | 0.82 | 1.94 |
| Burn the time (s) | GB/T14656-2009 | ≤60 | Not from putting out | 48 | 35 | 8 | 75 |
| Char length (mm) | GB/T14656-2009 | ≤115 | Not from putting out | 79 | 68 | 23 | 91 |
Annotate: press GB/T14656-2009, afterflame time≤5s burns time≤60s, and char length≤115 are fire retardant papers.
As can be seen from Table 1, the paper of the MgAlZnFe-LDHs preparation of rare earth element is not introduced in contrast, and the paper of introducing the LDHs preparation of rare earth element has significant flame retardant effect.
Claims (11)
1. one kind contains rare earth hydrotalcite fire retardant papers and its preparation method and application, it is characterized in that he composition and proportioning with paper fiber 100 listed as parts by weight, be specially:
100 parts of paper fibers
Contain 5 ~ 300 parts of rare earth hydrotalcites
The rare earth hydrotalcite fire retardant papers that contains according to claim 1 is characterized in that: it is characterized in that rear earth containing hydrotalcite of the present invention has following chemical formula: [M
2+ 1-x-yM
3+ xRe
3+ y(OH)
- 2] [A
n-]
X+y/nMH
2O, wherein Re is rare earth element.
2. form the common bivalent metal ion of LDHs Mg is arranged
2+, Zn
2+, Ni
2+, Co
2+, Cu
2+, Ca
2+, Mn
2+Common trivalent metal ion has A1
3+, Cr
3+, Co
3+, Fe
3+, Sc
3+, V
3+
3. by the rare earth hydrotalcite fire retardant papers that contains claimed in claim 1, it is characterized in that the trivalent rare earth CATION Re in described hydrotalcite
3+Refer to Eu
3+, Tb
3+, Sm
3+, Tm
3+, Ho
3+, Er
3+, Nd
3+, Pm
3+, Yb
3+, Lu
3+, Sc
3+, Y
3+, La
3+, Ce
3+, Pr
3+, Gd
3+Or Dy
3+
4. the rare earth hydrotalcite fire retardant papers that contains according to claim 1, is characterized in that: 0＜Re
3+/ [Re
3++ M
3+]≤0.5(mol ratio).
5. the rare earth hydrotalcite fire retardant papers that contains according to claim 1 is characterized in that: the mol ratio that in raw material, trivalent metal compound accounts for total metallic compound should satisfy 0.2≤(M
3++ Re
3+)/(M
2++ M
3++ Re
3+)≤0.3.
6. the rare earth hydrotalcite fire retardant papers that contains according to claim 1, it is characterized in that: hydrotalcite can be binary, ternary, quaternary, five yuan and the hexa-atomic rare earth hydrotalcite that contains.
7. the rare earth hydrotalcite fire retardant papers that contains according to claim 1, it is characterized in that: the hydrotalcite that adds can be organically-modified hydrotalcite, the modifier that uses can be odium stearate, dodecyl sodium sulfate, sodium hydrogen tartrate, itaconic acid, glycerin monostearate, silane coupler and polyethylene glycol, the consumption of modifier is 5 ~ 50 parts (quality), and method of modifying can be coprecipitation, ion-exchange or roasting restoring method.
8. the preparation method who contains rare earth hydrotalcite fire retardant papers according to claim 1 is characterized in that: under room temperature, salting liquid A and aqueous slkali B are added in the self-control reactor, the pH value of conditioned reaction liquid makes it remain at 8～11.
The question response drop complete after, being stirred a period of time in reactor after, the reactant liquor that obtains moves in there-necked flask, 80～100 ℃ of lower crystallization 4～8 h, then centrifugation, obtaining the LDHs filter cake with deionized water washing, is then the 1%-10%(mass fraction with the deionized water configuration concentration) LDHs colloidal solution.
10. getting a certain amount of absolute dried paper pulp discongests with deionized water in the standard fibre dissociation device and is made into suspension, then can directly adopt additive process in traditional slurry, infusion process and rubbing method will be above synthetic contain rare earth LDHs colloidal solution with paper pulp mixes, or employing molecular deposition, self-assembly method contain rare earth LDHs with paper fiber surface coating multilayer; The good paper fiber that will contain again rare earth LDHs modification is copied in sheet former and is obtained fire retardant papers.
11. the rare earth hydrotalcite fire retardant papers that contains according to claim 1 is characterized in that it can be used for the fields such as packing, building and paper for daily use.
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| CN103938487A (en) * | 2014-03-10 | 2014-07-23 | 王兆进 | Attapulgite clay fire retardation paper preparation method |
| CN105032440A (en) * | 2015-08-28 | 2015-11-11 | 齐鲁工业大学 | Zinc-copper-aluminum-erbium composite oxide as well as preparation method and application thereof |
| JPWO2018030521A1 (en) * | 2016-08-10 | 2018-08-09 | 日本製紙株式会社 | Hydrotalcite and fiber composite |
| JP2018172844A (en) * | 2016-08-10 | 2018-11-08 | 日本製紙株式会社 | Composite of hydrotalcite and fiber |
| JP6360638B2 (en) * | 2016-08-10 | 2018-07-18 | 日本製紙株式会社 | Hydrotalcite and fiber composite |
| JP2018090678A (en) * | 2016-11-30 | 2018-06-14 | 日本製紙株式会社 | Flame-retardant material |
| JP7065563B2 (en) | 2016-11-30 | 2022-05-12 | 日本製紙株式会社 | Flame-retardant material |
| CN109437115A (en) * | 2017-08-30 | 2019-03-08 | 上海沪正实业有限公司 | A kind of inorganic infrared barrier pigment and preparation method thereof |
| CN109695181A (en) * | 2017-10-20 | 2019-04-30 | 上海烟草集团有限责任公司 | A kind of cigarette paper and preparation method thereof with harm reduction function |
| CN109695181B (en) * | 2017-10-20 | 2021-07-09 | 上海烟草集团有限责任公司 | Cigarette paper with harm reducing function and preparation method thereof |
| CN108034265A (en) * | 2017-12-07 | 2018-05-15 | 常州帝君金属构件厂 | A kind of preparation method of flame-proof damp-proof type heat stabilizer |
| CN109112881A (en) * | 2018-09-03 | 2019-01-01 | 安庆市航海印务有限公司 | Anti-flaming dope is used in a kind of printing of paper products |
| CN111224049A (en) * | 2020-01-14 | 2020-06-02 | 江苏厚生新能源科技有限公司 | Flame-retardant lithium battery coating diaphragm and preparation method thereof |
| CN114656825A (en) * | 2022-03-09 | 2022-06-24 | 青岛爱尔家佳新材料股份有限公司 | Flame-retardant polyurea for new energy automobile and preparation method thereof |
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