CN107964829A - A kind of preparation method of high durable flame-proof paper - Google Patents
A kind of preparation method of high durable flame-proof paper Download PDFInfo
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- CN107964829A CN107964829A CN201711104736.3A CN201711104736A CN107964829A CN 107964829 A CN107964829 A CN 107964829A CN 201711104736 A CN201711104736 A CN 201711104736A CN 107964829 A CN107964829 A CN 107964829A
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- paper
- paper pulp
- parts
- pulp fiber
- magnalium hydrotalcite
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229920001131 Pulp (paper) Polymers 0.000 claims abstract description 84
- 239000000835 fiber Substances 0.000 claims abstract description 69
- 229910001051 Magnalium Inorganic materials 0.000 claims abstract description 43
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims abstract description 43
- 229960001545 hydrotalcite Drugs 0.000 claims abstract description 43
- 229910001701 hydrotalcite Inorganic materials 0.000 claims abstract description 43
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 39
- 239000000725 suspension Substances 0.000 claims description 28
- 238000012545 processing Methods 0.000 claims description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 22
- 238000001914 filtration Methods 0.000 claims description 20
- 238000001556 precipitation Methods 0.000 claims description 17
- 238000009938 salting Methods 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 15
- 238000001291 vacuum drying Methods 0.000 claims description 15
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 13
- 238000010494 dissociation reaction Methods 0.000 claims description 12
- 230000005593 dissociations Effects 0.000 claims description 12
- 238000002425 crystallisation Methods 0.000 claims description 11
- 230000008025 crystallization Effects 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical class [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 125000000129 anionic group Chemical group 0.000 claims description 9
- 239000003643 water by type Substances 0.000 claims description 9
- 238000009413 insulation Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000007792 addition Methods 0.000 claims description 7
- 239000003595 mist Substances 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 241000283216 Phocidae Species 0.000 claims description 6
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical class O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000013461 design Methods 0.000 claims description 6
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical class O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 5
- 238000011002 quantification Methods 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000004062 sedimentation Methods 0.000 claims description 2
- 238000000527 sonication Methods 0.000 claims description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims 1
- 125000002091 cationic group Chemical group 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 239000003063 flame retardant Substances 0.000 abstract description 34
- 230000000694 effects Effects 0.000 abstract description 7
- 230000014759 maintenance of location Effects 0.000 abstract description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 229920000620 organic polymer Polymers 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 230000005923 long-lasting effect Effects 0.000 abstract 1
- 239000000123 paper Substances 0.000 description 60
- 239000000243 solution Substances 0.000 description 14
- 239000000047 product Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000012757 flame retardant agent Substances 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-O phosphonium Chemical compound [PH4+] XYFCBTPGUUZFHI-UHFFFAOYSA-O 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/45—Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic Table; Aluminates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/285—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Paper (AREA)
Abstract
The present invention relates to fire retardant papers technical field of material, and in particular to a kind of preparation method of high durable flame-proof paper.Present invention self-control obtains magnalium hydrotalcite, filtered twice, copy paper, high durable flame-proof paper is obtained after drying, paper pulp fiber is after treatment, surface forms two-layer film configuration, enhance the electrostatic adsorption between magnalium hydrotalcite positive charge and paper pulp fiber negative electrical charge, so as to improve adhesive attraction of the magnalium hydrotalcite in paper pulp fiber, improve the retention of magnalium hydrotalcite, make the flame retardant effect of fire retardant papers more longlasting, polyacrylamide can greatly increase its steric hindrance, magnalium hydrotalcite surface positively charged, organic polymer polyacrylamide is negatively charged, magnalium hydrotalcite disperses evenly in paper pulp fiber, physics anchorage effect of the paper pulp fiber in magnalium hydrotalcite hole is stronger, so as to improve the retention of fire retardation magnalium hydrotalcite in fire retardant papers, improve its durability of fire-retardant energy, have a extensive future.
Description
Technical field
The present invention relates to fire retardant papers technical field of material, and in particular to a kind of preparation method of high durable flame-proof paper.
Background technology
Paper and paper products are most common articles in mankind's daily life, are usually manufactured paper with pulp and formed by plant fiber, belonged to
Combustible material.The inflammability of plant fiber, determines the inflammability of paper products.Due to the inflammability that it has, so usually can
Cause the generation of fire.In order to eliminate fire hazard, the research to paper products fire resistance is also growing day by day, the research of fire retardant papers
Also it has been continuously available the attention of people.
Fire retardant papers are that fire retardant is added to inside paper or is coated by the processing technology such as addition, dipping and coating in slurry
The paper surface prepared by.Fire retardant suppresses the generation of imflammable gas by hindering the thermal decomposition of fiber, or by every
Reach fire-retardant purpose from one or more of approach such as heat and air and dilution fuel gas.Fire retardant papers should possess following characteristic：
1st, the different flame-retardancy requirements that different product proposes can be met, its fire resistance cannot be decreased obviously because of the extension of time；2、
Used fire retardant decomposition temperature is suitable, cannot decompose in process, corrosion will not be caused to equipment and to ring
Border pollutes；3rd, the mechanical strength of fire retardant papers, colourity and other performances will be up to standard；4th, fire retardant papers will not in combustion process
Producing has human body and environment the gas of harm；5th, fire retardant is cheap, derives from a wealth of sources.
But also there is many deficiencies to need to improve for existing fire retardant papers, such as：When making fire retardant papers, amount of flame-retardant agent
Greatly, part product uses halogen phosphonium flame retardant, can damage to human body and environment；Fire retardant is readily volatilized, and the time is grown
Flame retardant effect will be decreased obviously, or even lose anti-flammability completely；The waterproof and dampproof property of fire retardant papers is poor, paper physical property after the moisture absorption
Decline etc..
Therefore, developing a kind of fire retardant papers that can solve above-mentioned performance issue is highly desirable.
The content of the invention
Present invention mainly solves technical problem, for fire retardant papers fire-retardant enduring quality it is poor the defects of, there is provided it is a kind of
The preparation method of high durable flame-proof paper.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of high durable flame-proof paper, it is characterised in that specifically preparation process is：
（1）Count in parts by weight, by 20~30 parts of Aluminum Chloride Hexahydrates and 10~15 parts of magnesium chloride hexahydrates be dissolved in 80~90 parts go from
In sub- water, salting liquid is obtained, 30~40 parts of sodium hydroxides and 30~35 parts of sodium carbonate are dissolved in 90~100 parts of deionized waters,
Aqueous slkali is obtained, aqueous slkali is put into supersonic wave cleaning machine with each self sealss of salting liquid and is ultrasonically treated；
（2）300~330mL salting liquids and 200~220mL aqueous slkalis are added dropwise to identical drop rate under nitrogen protection
In mist formula reactor processed, after completion of dropwise addition, start high speed agitator, stirring reaction, obtains reacting slurry；
（3）Reacting slurry is transferred in water-bath, heat temperature raising, insulation crystallization deposition, obtains crystallized precipitation, by crystallized precipitation
It is washed with deionized, the crystallized precipitation after washing is put into baking oven, heat temperature raising, it is dry, obtain magnalium hydrotalcite；
（4）Count in parts by weight, take 60~65 parts of absolute dried paper pulps to be put into standard dissociation device, deionization is added into standard dissociation device
Pulp suspension is separated by filtration to obtain negatively charged paper pulp fiber, configures magnesium until paper pulp is discongested as pulp suspension by water
Aluminum hydrotalcite suspension, paper fibre is immersed in 100~120 parts of magnalium hydrotalcite suspension, and stirring, is separated by filtration to obtain
The paper pulp fiber of first step processing, 80~90 parts of anionic polyacrylamide solution are put into by the paper pulp fiber of first step processing
In, stirring, is separated by filtration to obtain the paper pulp fiber of second step processing, and the paper pulp fiber of second step processing is put into and pours nitrogen
In baking oven, heat temperature raising is dry, obtains duplicature paper pulp fiber；
（5）Duplicature paper pulp fiber is mixed with deionized water, obtains paper pulp, paper pulp is put into the system of copying on quick sheet former
L Water Paper is obtained, l Water Paper is put into vacuum drying oven, vacuum drying obtains high durable flame-proof paper.
Step（1）Sonication treatment time is 15~20min in the supersonic wave cleaning machine, and control is cleaned by ultrasonic acc power
For 180~200W.
Step（2）The drop rate that controls is 8~10mL/min, and reactor system pH is 10~11, high-speed stirred
Device rotating speed is that the stirring reaction time is 30~35min.
Step（3）After the heat temperature raising temperature be 90~100 DEG C, insulation crystallization sedimentation time be 8~9h, spend from
Sub- water washing is until cleaning solution pH is 7.0~7.2, and temperature is 70~80 DEG C after heat temperature raising, and drying time is 20~24h.
Step（4）The mass fraction of the pulp suspension is 5%, and the mass concentration of magnalium hydrotalcite suspension is
10g/L's, the temperature of magnalium hydrotalcite suspension is 60~70 DEG C, and mixing time is 15~20min, anionic polyacrylamide
The temperature of solution is 70~80 DEG C, and the mass concentration of anionic polyacrylamide solution be 1g/mL, mixing time is 10~
15min, temperature is 80~90 DEG C after heat temperature raising, and drying time is 10~12h.
Step（5）The mass ratio that the duplicature paper pulp fiber is mixed with deionized water is 1:10, control l Water Paper quantifies
For 200~220g/m2, vacuum drying oven design temperature is 45~50 DEG C, and vacuum drying time is 6~10h.
The beneficial effects of the invention are as follows：
（1）The present invention with the aqueous slkali of the salting liquid of aluminium chloride and magnesium chloride, sodium hydroxide and sodium carbonate after supersound process,
Each instilled with identical drop speed in mist formula reactor processed, high-speed stirred obtains reacting slurry, and reacting slurry heats in water-bath
Crystallization, it is washed to be dried to obtain magnalium hydrotalcite, absolute dried paper pulp is put into magnalium hydrotalcite suspension, makes absolute dried paper pulp fiber
Electrostatic Absorption magnalium hydrotalcite, is obtained by filtration the paper pulp fiber of first step processing, places into adsorb in polyacrylamide solution and gathers
Acrylamide, is obtained by filtration the paper pulp fiber of second step processing, and after drying under a nitrogen, paper pulp is mixed to get with deionized water,
High durable flame-proof paper is dried to obtain after copy paper, for paper pulp fiber after two-step pretreatment, surface forms two-layer film configuration, two membranes band
Electric charge is different, enhances the electrostatic adsorption between magnalium hydrotalcite positive charge and paper pulp fiber negative electrical charge, makes to have fire-retardant
Retention improves during the magnalium hydrotalcite use of effect, and it is anti-that polyacrylamide can be catalyzed a variety of chemistry of hydroxyl on paper pulp fiber
Should, chemical reaction can make to rest on fiber or in the gap that fiber overlaps in a manner of being grafted containing magnalium hydrotalcite, so as to improve
Adhesive attraction of the magnalium hydrotalcite in paper pulp fiber, improves the retention of magnalium hydrotalcite, makes the flame retardant effect of fire retardant papers more
Persistently；
（2）Include substantial amounts of hydroxyl, absorption water and the crystallization water in the present invention in the interlayer and laminate of magnalium hydrotalcite, so
Adjacent nano magnalium hydrotalcite particle can be easily combined together because of the presence of hydrogen bond between each other in dehydration, be used
Polyacrylamide can replace the hydroxyl of magnalium hydrotalcite particle surface, greatly increase its steric hindrance, prevent from rolling into a ball between particle
Poly-, in addition magnalium hydrotalcite surface positively charged, organic polymer polyacrylamide are negatively charged, the two is tightly combined, and makes magnalium
Hydrotalcite disperses evenly in paper pulp fiber, and physics anchorage effect of the paper pulp fiber in magnalium hydrotalcite hole is stronger, from
And the retention of fire retardation magnalium hydrotalcite in fire retardant papers is improved, improve its durability of fire-retardant energy, have a extensive future.
Embodiment
Count in parts by weight, by 20~30 parts of Aluminum Chloride Hexahydrates and 10~15 parts of magnesium chloride hexahydrates be dissolved in 80~90 parts go from
In sub- water, salting liquid is obtained, 30~40 parts of sodium hydroxides and 30~35 parts of sodium carbonate are dissolved in 90~100 parts of deionized waters,
Aqueous slkali is obtained, aqueous slkali and each self sealss of salting liquid are put into 15~20min of supersound process in supersonic wave cleaning machine, control is super
Sound cleaning acc power is 180~200W；Under nitrogen protection by 300~330mL salting liquids and 200~220mL aqueous slkalis with phase
With drop rate be added dropwise in mist formula reactor processed, it is 8~10mL/min control drop rate, reactor system pH is 10~
11, after completion of dropwise addition, start high speed agitator, with rotating speed stirring 30~35min of reaction of 2000~2500r/min, obtain anti-
Answer slurries；Reacting slurry is transferred in water-bath, is heated to 90~100 DEG C, insulation crystallization deposits 8~9h, obtains crystalline substance
Change precipitation, crystallized precipitation is washed with deionized, until cleaning solution pH is 7.0~7.2, the crystallized precipitation after washing is put into
In baking oven, 70~80 DEG C are heated to, dry 20~24h, obtains magnalium hydrotalcite；Count in parts by weight, take 60~65 parts
Absolute dried paper pulp is put into standard dissociation device, and into standard dissociation device plus deionized water is until it is 5% that paper pulp, which is discongested as mass fraction,
Pulp suspension, pulp suspension is separated by filtration to obtain negatively charged paper pulp fiber, configuration quality concentration is the magnesium of 10g/L
Aluminum hydrotalcite suspension, is immersed in 100~120 parts of temperature in 60~70 DEG C of magnalium hydrotalcite suspension, to stir by paper fibre
15~20min is mixed, is separated by filtration to obtain the paper pulp fiber of first step processing, the paper pulp fiber of first step processing is put into 80~90
Part temperature is in the anionic polyacrylamide solution that 70~80 DEG C of mass concentrations are 1g/mL, stirs 10~15min, filtering point
From the paper pulp fiber of second step processing is obtained, the paper pulp fiber of second step processing is put into the baking oven for pouring nitrogen, heating rises
For temperature to 80~90 DEG C, dry 10~12h, obtains duplicature paper pulp fiber；Duplicature paper pulp fiber and deionized water are pressed into quality
Than for 1:10 mixing, obtain paper pulp, paper pulp are put into copy on quick sheet former l Water Paper is made, and control l Water Paper is quantification of
200~220g/m2, l Water Paper is put into the vacuum drying oven that design temperature is 45~50 DEG C, 6~10h of vacuum drying obtains high resistance to
Long fire retardant papers.
Example 1
Count in parts by weight, 20 parts of Aluminum Chloride Hexahydrates and 10 parts of magnesium chloride hexahydrates are dissolved in 80 parts of deionized waters, it is molten to obtain salt
Liquid, 30 parts of sodium hydroxides and 30 parts of sodium carbonate are dissolved in 90 parts of deionized waters, obtain aqueous slkali, and aqueous slkali is each with salting liquid
Self sealss, which are put into supersonic wave cleaning machine, is ultrasonically treated 15min, and it is 180W to control ultrasonic cleaning acc power；Under nitrogen protection will
300mL salting liquids and 200mL aqueous slkalis are added dropwise in mist formula reactor processed with identical drop rate, control the drop rate to be
8mL/min, reactor system pH are 10, after completion of dropwise addition, start high speed agitator, and reaction is stirred with the rotating speed of 2000r/min
30min, obtains reacting slurry；Reacting slurry is transferred in water-bath, is heated to 90 DEG C, insulation crystallization deposition 8h, obtains
To crystallized precipitation, crystallized precipitation is washed with deionized, until cleaning solution pH is 7.0, the crystallized precipitation after washing is put into
In baking oven, 70 DEG C are heated to, dry 20h, obtains magnalium hydrotalcite；Count in parts by weight, take 60 parts of absolute dried paper pulps to be put into
In standard dissociation device, into standard dissociation device plus deionized water until paper pulp discongest the pulp suspension for being 5% for mass fraction,
Pulp suspension is separated by filtration to obtain negatively charged paper pulp fiber, configuration quality concentration is that the magnalium hydrotalcite of 10g/L hangs
Supernatant liquid, is immersed in 100 parts of temperature in 60 DEG C of magnalium hydrotalcite suspension, to stir 15min, being separated by filtration to obtain by paper fibre
The paper pulp fiber of first step processing, it is that 70 DEG C of mass concentrations are 1g/mL that the paper pulp fiber of first step processing is put into 80 parts of temperature
Anionic polyacrylamide solution in, stir 10min, be separated by filtration to obtain the paper pulp fiber of second step processing, by second step
The paper pulp fiber of processing is put into the baking oven for pouring nitrogen, is heated to 80 DEG C, dry 10h, obtains duplicature paper pulp fiber；
It is 1 in mass ratio by duplicature paper pulp fiber and deionized water:10 mixing, obtain paper pulp, paper pulp are put into quick paper sheet formation
Copied on device and l Water Paper is made, the quantification of 200g/m of control l Water Paper2, l Water Paper is put into the vacuum drying oven that design temperature is 45 DEG C,
Vacuum drying 6h obtains high durable flame-proof paper.
Example 2
Count in parts by weight, 25 parts of Aluminum Chloride Hexahydrates and 13 parts of magnesium chloride hexahydrates are dissolved in 85 parts of deionized waters, it is molten to obtain salt
Liquid, 35 parts of sodium hydroxides and 32 parts of sodium carbonate are dissolved in 95 parts of deionized waters, obtain aqueous slkali, and aqueous slkali is each with salting liquid
Self sealss, which are put into supersonic wave cleaning machine, is ultrasonically treated 17min, and it is 190W to control ultrasonic cleaning acc power；Under nitrogen protection will
315mL salting liquids and 210mL aqueous slkalis are added dropwise in mist formula reactor processed with identical drop rate, control the drop rate to be
9mL/min, reactor system pH are 10.5, after completion of dropwise addition, start high speed agitator, anti-with the rotating speed stirring of 2250r/min
33min is answered, obtains reacting slurry；Reacting slurry is transferred in water-bath, is heated to 95 DEG C, insulation crystallization deposition
8.5h, obtains crystallized precipitation, and crystallized precipitation is washed with deionized, until cleaning solution pH is 7.1, the crystallization after washing is sunk
Shallow lake is put into baking oven, is heated to 75 DEG C, dry 23h, obtains magnalium hydrotalcite；Count in parts by weight, take 63 parts of bone-dry papers
Slurry is put into standard dissociation device, and into standard dissociation device plus deionized water is until paper pulp is discongested the paper pulp for being 5% for mass fraction and hanged
Supernatant liquid, pulp suspension is separated by filtration to obtain negatively charged paper pulp fiber, configuration quality concentration is the magnalium neatly of 10g/L
Stone suspension, is immersed in 110 parts of temperature in 65 DEG C of magnalium hydrotalcite suspension, to stir 17min, being separated by filtration by paper fibre
The paper pulp fiber of first step processing is obtained, it is that 75 DEG C of mass concentrations are that the paper pulp fiber of first step processing is put into 85 parts of temperature
In the anionic polyacrylamide solution of 1g/mL, 13min is stirred, is separated by filtration to obtain the paper pulp fiber of second step processing, by the
The paper pulp fiber of two steps processing is put into the baking oven for pouring nitrogen, is heated to 85 DEG C, dry 11h, obtains duplicature paper pulp
Fiber；It is 1 in mass ratio by duplicature paper pulp fiber and deionized water:10 mixing, obtain paper pulp, paper pulp are put into quick page
Copied on former and l Water Paper is made, the quantification of 210g/m of control l Water Paper2, l Water Paper is put into the vacuum drying oven that design temperature is 48 DEG C
In, vacuum drying 8h obtains high durable flame-proof paper.
Example 3
Count in parts by weight, 30 parts of Aluminum Chloride Hexahydrates and 15 parts of magnesium chloride hexahydrates are dissolved in 90 parts of deionized waters, it is molten to obtain salt
Liquid, 40 parts of sodium hydroxides and 35 parts of sodium carbonate are dissolved in 100 parts of deionized waters, obtain aqueous slkali, by aqueous slkali and salting liquid
Each self sealss, which are put into supersonic wave cleaning machine, is ultrasonically treated 20min, and it is 200W to control ultrasonic cleaning acc power；Under nitrogen protection
330mL salting liquids and 220mL aqueous slkalis are added dropwise in mist formula reactor processed with identical drop rate, control the drop rate to be
10mL/min, reactor system pH are 11, after completion of dropwise addition, start high speed agitator, and reaction is stirred with the rotating speed of 2500r/min
35min, obtains reacting slurry；Reacting slurry is transferred in water-bath, is heated to 100 DEG C, insulation crystallization deposition 9h, obtains
To crystallized precipitation, crystallized precipitation is washed with deionized, until cleaning solution pH is 7.2, the crystallized precipitation after washing is put into
In baking oven, 80 DEG C are heated to, dry 24h, obtains magnalium hydrotalcite；Count in parts by weight, take 65 parts of absolute dried paper pulps to be put into
In standard dissociation device, into standard dissociation device plus deionized water until paper pulp discongest the pulp suspension for being 5% for mass fraction,
Pulp suspension is separated by filtration to obtain negatively charged paper pulp fiber, configuration quality concentration is that the magnalium hydrotalcite of 10g/L hangs
Supernatant liquid, is immersed in 120 parts of temperature in 70 DEG C of magnalium hydrotalcite suspension, to stir 20min, being separated by filtration to obtain by paper fibre
The paper pulp fiber of first step processing, it is that 80 DEG C of mass concentrations are 1g/mL that the paper pulp fiber of first step processing is put into 90 parts of temperature
Anionic polyacrylamide solution in, stir 15min, be separated by filtration to obtain the paper pulp fiber of second step processing, by second step
The paper pulp fiber of processing is put into the baking oven for pouring nitrogen, is heated to 90 DEG C, dry 12h, obtains duplicature paper pulp fiber；
It is 1 in mass ratio by duplicature paper pulp fiber and deionized water:10 mixing, obtain paper pulp, paper pulp are put into quick paper sheet formation
Copied on device and l Water Paper is made, the quantification of 220g/m of control l Water Paper2, l Water Paper is put into the vacuum drying oven that design temperature is 50 DEG C,
Vacuum drying 10h obtains high durable flame-proof paper.
Comparative example
With the fire retardant papers of company of Suzhou City production as a comparison case in high durable flame-proof paper produced by the present invention and comparative example
Fire retardant papers be detected, testing result is as shown in table 1：1st, test method
Testing index uses《Fire retardant papers and cardboard combustibility test method》（GB/T14656-2009）Standard performs.
Table 1
| Test event | Example 1 | Example 2 | Example 3 | Comparative example |
| Heat release rate peak value（kW/m2） | 40.3 | 40.0 | 39.5 | 70.6 |
| Mass loss rate（cm3/g） | 58.9 | 58.4 | 58.1 | 75.9 |
| Limited oxygen index（%） | 38 | 40 | 41 | 30 |
| Horizontal firing length（mm） | 4 | 4 | 3 | 20 |
| The vertical combustion time（s） | 0 | 0 | 0 | 2 |
| Limited oxygen index（%）/（Room temperature preservation 2 years） | 36 | 37 | 38 | 25 |
From the data in table 1, it can be seen that high durable flame-proof paper produced by the present invention, fire resistance is good, smoke suppressing effect is good.Therefore, have wide
Wealthy prospect of the application.
Claims (6)
1. a kind of preparation method of high durable flame-proof paper, it is characterised in that specifically preparation process is：
（1）Count in parts by weight, by 20~30 parts of Aluminum Chloride Hexahydrates and 10~15 parts of magnesium chloride hexahydrates be dissolved in 80~90 parts go from
In sub- water, salting liquid is obtained, 30~40 parts of sodium hydroxides and 30~35 parts of sodium carbonate are dissolved in 90~100 parts of deionized waters,
Aqueous slkali is obtained, aqueous slkali is put into supersonic wave cleaning machine with each self sealss of salting liquid and is ultrasonically treated；
（2）300~330mL salting liquids and 200~220mL aqueous slkalis are added dropwise to identical drop rate under nitrogen protection
In mist formula reactor processed, after completion of dropwise addition, start high speed agitator, stirring reaction, obtains reacting slurry；
（3）Reacting slurry is transferred in water-bath, heat temperature raising, insulation crystallization deposition, obtains crystallized precipitation, by crystallized precipitation
It is washed with deionized, the crystallized precipitation after washing is put into baking oven, heat temperature raising, it is dry, obtain magnalium hydrotalcite；（4）
Count in parts by weight, take 60~65 parts of absolute dried paper pulps to be put into standard dissociation device, into standard dissociation device plus deionized water until
Paper pulp is discongested as pulp suspension, and pulp suspension is separated by filtration to obtain negatively charged paper pulp fiber, configures magnalium neatly
Stone suspension, paper fibre is immersed in 100~120 parts of magnalium hydrotalcite suspension, and stirring, is separated by filtration to obtain the first step
The paper pulp fiber of processing, the paper pulp fiber of first step processing is put into 80~90 parts of anionic polyacrylamide solution, is stirred,
It is separated by filtration to obtain the paper pulp fiber of second step processing, the paper pulp fiber of second step processing is put into the baking oven for pouring nitrogen,
Heat temperature raising, it is dry, obtain duplicature paper pulp fiber；
（5）Duplicature paper pulp fiber is mixed with deionized water, obtains paper pulp, paper pulp is put into the system of copying on quick sheet former
L Water Paper is obtained, l Water Paper is put into vacuum drying oven, vacuum drying obtains high durable flame-proof paper.
A kind of 2. preparation method of high durable flame-proof paper according to claim 1, it is characterised in that：Step（1）Described
Sonication treatment time is 15~20min in supersonic wave cleaning machine, and it is 180~200W to control ultrasonic cleaning acc power.
A kind of 3. preparation method of high durable flame-proof paper according to claim 1, it is characterised in that：Step（2）Described
It is 8~10mL/min to control drop rate, and reactor system pH is 10~11, and high speed agitator rotating speed is to stir the reaction time
For 30~35min.
A kind of 4. preparation method of high durable flame-proof paper according to claim 1, it is characterised in that：Step（3）Described
Temperature is 90~100 DEG C after heat temperature raising, and insulation crystallization sedimentation time is 8~9h, is washed with deionized until cleaning solution pH
For 7.0~7.2, temperature is 70~80 DEG C after heat temperature raising, and drying time is 20~24h.
A kind of 5. preparation method of high durable flame-proof paper according to claim 1, it is characterised in that：Step（4）Described
The mass fraction of pulp suspension is 5%, and the mass concentration of magnalium hydrotalcite suspension is 10g/L, magnalium hydrotalcite suspension
Temperature be 60~70 DEG C, mixing time be 15~20min, and the temperature of anionic polyacrylamide solution is 70~80 DEG C, the moon
The mass concentration of cationic polyacrylamide solution is 1g/mL, and mixing time is 10~15min, after heat temperature raising temperature for 80~
90 DEG C, drying time is 10~12h.
A kind of 6. preparation method of high durable flame-proof paper according to claim 1, it is characterised in that：Step（5）Described
The mass ratio that duplicature paper pulp fiber is mixed with deionized water is 1:10, the quantification of 200~220g/m of control l Water Paper2, vacuum baking
Case design temperature is 45~50 DEG C, and vacuum drying time is 6~10h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109162148A (en) * | 2018-09-20 | 2019-01-08 | 何治伟 | A kind of preparation method of primary composite modified fire retardant papers material |
| CN109989294A (en) * | 2019-03-29 | 2019-07-09 | 潍坊科技学院 | A kind of preparation method of organically-modified hydrotalcite Flame Retardant in Paper |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351225A (en) * | 2011-07-06 | 2012-02-15 | 北京科技大学 | Method for preparing chloride ion treating medicament |
| CN104532659A (en) * | 2014-12-02 | 2015-04-22 | 王庆艳 | Highly filled flame-retardant paper and preparation method thereof |
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2017
- 2017-11-10 CN CN201711104736.3A patent/CN107964829A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351225A (en) * | 2011-07-06 | 2012-02-15 | 北京科技大学 | Method for preparing chloride ion treating medicament |
| CN104532659A (en) * | 2014-12-02 | 2015-04-22 | 王庆艳 | Highly filled flame-retardant paper and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109162148A (en) * | 2018-09-20 | 2019-01-08 | 何治伟 | A kind of preparation method of primary composite modified fire retardant papers material |
| CN109989294A (en) * | 2019-03-29 | 2019-07-09 | 潍坊科技学院 | A kind of preparation method of organically-modified hydrotalcite Flame Retardant in Paper |
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Application publication date: 20180427 |