CN110359120A - A kind of preparation method of melamine modified urea-formaldehyde fiber - Google Patents
A kind of preparation method of melamine modified urea-formaldehyde fiber Download PDFInfo
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- CN110359120A CN110359120A CN201910694132.1A CN201910694132A CN110359120A CN 110359120 A CN110359120 A CN 110359120A CN 201910694132 A CN201910694132 A CN 201910694132A CN 110359120 A CN110359120 A CN 110359120A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08G12/34—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds and acyclic or carbocyclic compounds
- C08G12/36—Ureas; Thioureas
- C08G12/38—Ureas; Thioureas and melamines
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
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Abstract
The invention discloses a kind of preparation methods of melamine modified urea-formaldehyde fiber, and melamine and aldehydes (first solution), urea and aldehydes (second solution) are separately added into two parts of water-soluble polymers, are separately added into basic catalyst reaction different time；Acidic catalyst is added in the mixing of first, second solvent, and the reaction was continued, again plus basic catalyst and the reaction of remaining aldehyde compound, after using wet-spinning frame carry out spinning, by coagulating bath wind as-spun fibre be heating and curing in an oven, after Temperature fall take out obtain modified urea-formaldehyde fiber.The present invention is prepared for modified urea-formaldehyde fiber by rationally designing reaction process, wet spinning, which has many advantages, such as that at low cost, flame-retardant fiber, heat-insulated, nothing melt drop, burn nontoxic, have broad application prospects as three-dimensional cross-linked fiber type.
Description
Technical field
The invention belongs to the preparation fields of special fibre, and in particular to a kind of melamine modified urea-formaldehyde spinning solution system
Standby, wet spinning and heat cure are to obtain the preparation method of modified urea-formaldehyde fiber.
Background technique
Three-dimensional cross-linked fiber type have the characteristics that it is intrinsic it is fire-retardant, it is heat-insulated and carbonization yield it is high in functional textile, carbon fiber
Dimension and activated carbon fibre field have potential application.But since cross-linked fiber has different preparations from orientation fiber
Method and structure feature, so that the development of cross-linked fiber is extremely slow.
Phenolic fibre is the first three-dimensional cross-linked organic fiber [ Economy J, Clark R A.US patent,
3650102 ], the appearance of the fiber broken three-dimensional cross-linked resin can not be at fine intrinsic notion.Melamine passes through with formaldehyde
The tridimensional network that condensation reaction is formed assigns the performances such as the good fire-retardant, acid and alkali-resistance of melamine resin fiber, high temperature resistant.
Melamine resin (MF) fiber is also known as melamine fiber, is to have a kind of cross filament after phenolic fibre.With good resistance
Combustion property, limit oxygen index burn or generate with when flame contact without toxic gas up to 32；It is not melted in combustion process, without drop
It falls, can avoid spot fire；Melamine fiber can be used for a long time under the conditions of 200 DEG C simultaneously, and size, tensile strength are almost without change
Change [Luo Yifeng.New developments in hi-tech synthetic fibers [J].Tec fiber and application, 2000 (4): 1-8], melamine fiber can be
It is carbonized, activates under higher temperature, prepare carbon fiber or porous carbon fiber material.Melamine fiber can be widely applied to fire-retardant weaving
The fields such as product, high temperature filtration, purification absorption.
Lauxite is widely used in manufacture furniture appliance, machine components, electrically as urea-formaldehyde plastics, wood adhesive etc.
Accessory, various button and cover board etc. are rapidly progressed due to cheap, good flame resistance, but answering in terms of fiber
With having no relevant report.The advantages of both present invention combination ureaformaldehyde, melamine, it is prepared for modified urea-formaldehyde fiber.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of melamine modified urea-formaldehyde fiber, water-soluble in two parts of macromolecules
It is blended after melamine, urea and aldehyde compound reaction are added in liquid, after undergoing acid reaction process, is adjusted to alkali again
Property condition, remaining aldehyde compound, which is added, to react to obtain spinning solution, and wet spinning, heat cure prepare three-dimensional cross-linked modification
Ureaformaldehyde fiber.This method provides a kind of preparation methods of melamine modified urea-formaldehyde fiber.
The technical scheme is that a kind of preparation method of melamine modified urea-formaldehyde fiber, steps are as follows:
(1) water soluble polymer aqueous solution is obtained by water soluble polymer is soluble in water, by water soluble polymer aqueous solution equal part
At A, B two parts, melamine, aldehydes and basic catalyst are added into part A solution, is reacted under the conditions of 50-95 DEG C
0.4-10h obtains first solution；Urea and aldehyde compound and basic catalyst are added into part B solution, then in 45-
0.5-8h is reacted under the conditions of 95 DEG C, obtains second solution；PH value is adjusted after the mixing of first, second solution to acidity, under the conditions of 40-95 DEG C
The reaction was continued 0.1-7h, obtains modified urea-formaldehyde resin solution；
(2) basic catalyst is added and adjusts modified urea-formaldehyde resin solution to alkalinity, and is slowly added to aldehyde compound, in 35-95
After reacting a period of time under the conditions of DEG C, modified urea-formaldehyde spinning solution is obtained, using wet spinning technology, is obtained after coagulating bath
Ureaformaldehyde as-spun fibre；
(3) then as-spun fibre is heating and curing in an oven according to certain heating rate, obtains by washing, drying
Modified urea-formaldehyde fiber.
Further, water soluble polymer is PVA, PEG in the step (1), polyvinyl formal, PVP, water solubility change
Property one of starch or water-soluble modified cellulose；High molecular mass content is 1-30% in water soluble polymer aqueous solution.
Further, the aldehyde compound is one of formaldehyde, glutaraldehyde, acetaldehyde, paraformaldehyde；Basic catalyst is
One of sodium hydroxide, potassium hydroxide, triethanolamine, sodium bicarbonate, magnesium hydroxide or calcium hydroxide, acidic catalyst are salt
One of acid, sulfuric acid, phosphoric acid or oxalic acid.
Further, in step (1) the part A solution, the molar ratio of melamine and aldehydes is 1:(0.7-1.9), it is high
The mass ratio of molecule and melamine is 1:(0.1-4)；The molar ratio of urea and aldehydes is 1:0.7-1.9 in part B solution, high
The mass ratio of molecule and urea is 1:(0.2-10).
Further, the pH value range of first solution is 7.4-11 in the step (1), and the pH value range of second solution is 7.5-
10.5, it is 4.0-6.9 that pH value range is adjusted after the mixing of first, second solution.
Further, it is 7.4-10.5 that basic catalyst is added in the step (2) and adjusts urea-formaldehyde resin solution pH value range,
Reaction time is 0.4-8h.
Further, the additional amount of step (2) aldehyde compound is on the basis of urea in step (1), urea and aldehydes
The mass ratio of the material of compound is 1:(0.3-2).
Further, the coagulating bath of wet spinning is saturated aqueous sodium sulfate in the step (2), and adds weight content
For the boric acid of 0.1-5%, temperature is 10-60 DEG C, winding speed 10-500m/min.
Further, 20-40 DEG C of drying temperature in vacuum drying oven of as-spun fibre, heating rate 1- in the step (3)
30 DEG C/min, it is warming up to 150-230 DEG C, constant temperature 0.1-2h, is taken out after Temperature fall up to modified urea-formaldehyde fiber.
The invention has the following advantages: urea and aldehyde compound raw material are cheap and easy to get, it is not necessarily to strong acid, highly basic or corruption
Corrosion condition, reaction condition are mild；The addition of melamine improves the degree of functionality of molecule, is conducive to and aldehyde reaction, reduction are swum
From aldehyde, mechanical property is improved；Ureaformaldehyde molecule is the linear structure of high molecular weight in gained spinning solution, is had higher viscous
Degree, excellent spinnability, without be further processed can direct fabrics, spinning condition is mild, and spinning speed is fast, gained as-spun fibre
Only need to be by heat cure up to modified urea-formaldehyde fiber, solidification crosslinking is simple and easy；Gained modified urea-formaldehyde fiber is a kind of three-dimensional friendship
Join fiber, without adding fire retardant, excellent flame retardancy, limit oxygen index is high, discharges poisonous and harmful gas when putting out, burning from flame
Body is considerably less, and flame-retarding is high, and heat-proof quality is excellent, and fibrous mechanical property increases.
Specific embodiment
The present invention will be further explained with reference to the examples below, as described below, is only to preferable implementation of the invention
Example, not limits the present invention, any person skilled in the art is possibly also with the disclosure above
Technology contents be changed to the equivalent embodiment changed on an equal basis.Without departing from the concept of the present invention, according to the present invention
Technical spirit any simple modification or equivalent variations that following embodiment is made, fall within the scope of protection of the present invention.
Embodiment 1
The preparation method of the melamine modified urea-formaldehyde fiber of the present embodiment, steps are as follows:
(1) by the PVA PVA aqueous solution soluble in water for obtaining 1wt%, two parts are divided into, melamine, acetaldehyde is added in a part
And potassium hydroxide, 0.4h is reacted under the conditions of pH is 7.4,50 DEG C, and the molar ratio of melamine and acetaldehyde is 1:0.7, wherein PVA
Mass ratio with melamine is 1:0.1；Urea and formaldehyde (molar ratio 1:0.7) is added in another part, wherein PVA and urea
Mass ratio be 1:0.2；Then sodium hydrate aqueous solution is added, adjusts pH value to 7.5, in 45 DEG C of reaction 0.5h；Two parts are molten
Salt acid for adjusting pH value is added to 4.0,40 DEG C of reaction 0.1h in liquid after being blended；
(2) calcium hydroxide aqueous solution is added again, adjusts pH value to 7.4, paraformaldehyde is then added and (urine is added in step (1)
The mass ratio of the material of element and paraformaldehyde is 1:0.3), it is molten to obtain the modified urea-formaldehyde that aldehyde is 0.09% by 35 DEG C of reaction 0.4h
Liquid；
(3) gained spinning solution is by wet spinning, use saturated aqueous sodium sulfate that weight content is 0.1% boric acid as
Coagulating bath, winding speed is that 10m/min obtains as-spun fibre at 10 DEG C of temperature, then after 20 DEG C of drying, is heated up with 1 DEG C/min
It 150 DEG C, constant temperature 0.1h, takes out after Temperature fall up to modified urea-formaldehyde fiber.
The modified urea-formaldehyde fibre diameter of preparation is 11 microns, tensile strength 354MPa, elongation at break 30%, fiber
LOI value be 33.
Embodiment 2
The preparation method of the melamine modified urea-formaldehyde fiber of the present embodiment, steps are as follows:
(1) by the PEG PEG aqueous solution soluble in water for obtaining 30wt%, two parts are divided into, melamine, formaldehyde is added in a part
And sodium hydroxide, 10h is reacted under the conditions of pH is 11,95 DEG C, and the molar ratio of melamine and formaldehyde is 1:1.9, wherein PEG
Mass ratio with melamine is 1:4；Urea and paraformaldehyde (molar ratio 1:1.9) is added in another part, wherein PEG with
The mass ratio of urea is 1:10；Then potassium hydroxide aqueous solution is added, adjusts pH value to 10.5, in 95 DEG C of reaction 8h；Two parts
Sulphur acid for adjusting pH value is added after solution blending to 6.9,95 DEG C of reaction 7h；
(2) be added sodium hydrate aqueous solution again, adjust pH value to 10.5, be then added formaldehyde (be added in step (1) urea and
The mass ratio of the material of formaldehyde is 1:2), 95 DEG C of reaction 8h obtain the modified urea-formaldehyde solution that aldehyde is 0.08%；
(3) gained spinning solution is by wet spinning, uses saturated aqueous sodium sulfate that weight content is 5% boric acid as coagulating
Gu bathing, winding speed is that 500m/min obtains as-spun fibre under temperature 60 C, then after 40 DEG C of dryings, with 30 DEG C/min heating
It 230 DEG C, constant temperature 2h, takes out after Temperature fall up to ureaformaldehyde fiber.
The ureaformaldehyde fibre diameter of preparation is 20 microns, tensile strength 336MPa, elongation at break 15%, the LOI of fiber
Value is 31.
Embodiment 3
The preparation method of the melamine modified urea-formaldehyde fiber of the present embodiment, steps are as follows:
(1) by the polyvinyl formal polyvinyl formal solution soluble in water for obtaining 20wt%, two parts are divided into,
Melamine, glutaraldehyde and calcium hydroxide is added in a part, reacts 4h, melamine and penta 2 under the conditions of pH is 8.5,65 DEG C
The molar ratio of aldehyde is 1:1.3；Wherein the mass ratio of polyvinyl formal melamine is 1:3；Another part be added urea and
Glutaraldehyde (molar ratio 1:1.1), wherein the mass ratio of polyvinyl formal and urea is 1:5；Then triethanolamine is added,
PH value is adjusted to 8.5, in 90 DEG C of reaction 3h；Phosphorus acid for adjusting pH value is added after two parts solution blending to 5,85 DEG C of reaction 2h；
(2) be added potassium hydroxide aqueous solution again, adjust pH value to 8.5, be then added acetaldehyde (be added in step (1) urea and
The mass ratio of the material of acetaldehyde is 1:0.5), 75 DEG C of reaction 4h obtain the modified urea-formaldehyde solution that aldehyde is 0.1%；
(3) gained spinning solution is by wet spinning, uses saturated aqueous sodium sulfate that weight content is 3% boric acid as coagulating
Gu bathing, winding speed is that 300m/min obtains as-spun fibre under temperature 50 C, then after 30 DEG C of dryings, with 20 DEG C/min heating
It 210 DEG C, constant temperature 1h, takes out after Temperature fall up to modified urea-formaldehyde fiber.
The modified urea-formaldehyde fibre diameter of preparation is 30 microns, tensile strength 280MPa, elongation at break 25%, fiber
LOI value be 32.
Embodiment 4
The preparation method of the melamine modified urea-formaldehyde fiber of the present embodiment, steps are as follows:
(1) by the PVP PVP aqueous solution soluble in water for obtaining 10wt%, two parts are divided into, melamine, poly is added in a part
Formaldehyde and magnesium hydroxide react 3h under the conditions of pH is 9,55 DEG C, and the molar ratio of melamine and paraformaldehyde is 1:1.1,
The mass ratio of middle PVP and melamine is 1:0.2；Urea and acetaldehyde (molar ratio 1:1.1) is added in another part, wherein PVP
Mass ratio with urea is 1:3；Then sodium bicarbonate is added, adjusts pH value to 8.5, in 90 DEG C of reaction 2h；Two parts solution is total
Careless acid for adjusting pH value is added after mixed to 5.5,85 DEG C of reaction 2h；
(2) it is added triethanolamine again, adjusts pH value to 8.5, paraformaldehyde is then added and (urea and more is added in step (1)
The mass ratio of the material of polyformaldehyde is 1:0.5), 75 DEG C of reaction 4h obtain the modified urea-formaldehyde solution that aldehyde is 0.12%；
(3) gained spinning solution is by wet spinning, uses saturated aqueous sodium sulfate that weight content is 3% boric acid as coagulating
Gu bathing, winding speed is that 200m/min obtains as-spun fibre under temperature 50 C, then after 30 DEG C of dryings, with 20 DEG C/min heating
It 180 DEG C, constant temperature 1h, takes out after Temperature fall up to modified urea-formaldehyde fiber.
The modified urea-formaldehyde fibre diameter of preparation is 19 microns, tensile strength 310MPa, elongation at break 19%, fiber
LOI value be 34.
Embodiment 5
The preparation method of the melamine modified urea-formaldehyde fiber of the present embodiment, steps are as follows:
(1) by the water soluble starch water soluble starch aqueous solution soluble in water for obtaining 10wt%, two parts are divided into, a part adds
Enter melamine, formaldehyde and sodium bicarbonate, react 5h under the conditions of pH is 9.1,75 DEG C, the molar ratio of melamine and formaldehyde is
1:0.9, wherein the mass ratio of water soluble starch and melamine is 1:0.2；Another part be added urea and paraformaldehyde (mole
Than for 1:1.1), wherein the mass ratio of water soluble starch and urea is 1:0.5；Then magnesium hydroxide is added, adjusts pH value and arrives
8.5, in 90 DEG C of reaction 2h；Sulphur acid for adjusting pH value is added after two parts solution blending to 5.5,85 DEG C of reaction 2h；
(2) sodium bicarbonate is added again, adjusts pH value to 8.5, glutaraldehyde is then added and (urea and penta 2 is added in step (1)
The mass ratio of the material of aldehyde is 1:0.5), 75 DEG C of reaction 4h obtain the modified urea-formaldehyde solution that aldehyde is 0.06%；
(3) gained spinning solution is by wet spinning, uses saturated aqueous sodium sulfate that weight content is 2% boric acid as coagulating
Gu bathing, winding speed is that 180m/min obtains as-spun fibre at 40 DEG C of temperature, then after 30 DEG C of dryings, with 20 DEG C/min heating
It 190 DEG C, constant temperature 1h, takes out after Temperature fall up to modified urea-formaldehyde fiber.
The modified urea-formaldehyde fibre diameter of preparation is 28 microns, tensile strength 230MPa, elongation at break 19%, fiber
LOI value be 33.
Embodiment 6
The preparation method of the melamine modified urea-formaldehyde fiber of the present embodiment, steps are as follows:
(1) two parts are divided by the water-soluble cellulose water-soluble cellulose aqueous solution soluble in water for obtaining 18wt%, one
Divide and melamine, paraformaldehyde and triethanolamine is added, reacts 0.9h, melamine and poly under the conditions of pH is 8.0,85 DEG C
The molar ratio of formaldehyde is 1:1.2；Wherein the mass ratio of water-soluble cellulose and melamine is 1:1；Urea is added in another part
With glutaraldehyde (molar ratio 1:1.2), wherein the mass ratio of water-soluble cellulose and urea is 1:2；Then calcium hydroxide is added,
PH value is adjusted to 8.5, in 90 DEG C of reaction 2h；Sulphur acid for adjusting pH value is added after two parts solution blending to 5.5,85 DEG C of reaction 3h；
(2) it is added magnesium hydroxide again, adjusts pH value to 8.5, formaldehyde is then added and (urea and formaldehyde are added in step (1)
The mass ratio of the material is 1:0.8), 75 DEG C of reaction 4h obtain the modified urea-formaldehyde solution that aldehyde is 0.1%；
(3) gained spinning solution is by wet spinning, use saturated aqueous sodium sulfate that weight content is 0.9% boric acid as
Coagulating bath, winding speed is that 50m/min obtains as-spun fibre at 40 DEG C of temperature, then after 30 DEG C of drying, is heated up with 20 DEG C/min
It 190 DEG C, constant temperature 1h, takes out after Temperature fall up to modified urea-formaldehyde fiber.
The modified urea-formaldehyde fibre diameter of preparation is 28 microns, tensile strength 280MPa, elongation at break 30%, fiber
LOI value be 31.
Embodiment 7
The preparation method of the melamine modified urea-formaldehyde fiber of the present embodiment, steps are as follows:
(1) two parts are divided by the water-soluble cellulose water-soluble cellulose aqueous solution soluble in water for obtaining 18wt%, one
Point melamine, acetaldehyde and potassium hydroxide is added, reacts 4.5h under the conditions of pH is 10,80 DEG C, melamine and acetaldehyde rub
You are than being 1:1, and wherein the mass ratio of water-soluble cellulose and melamine is 1:0.4；Urea and formaldehyde is added in another part
(molar ratio 1:1.2), wherein the mass ratio of water-soluble cellulose and urea is 1:3；Then sodium hydroxide is added, adjusts pH value
To 8.5, in 90 DEG C of reaction 2h；Careless acid for adjusting pH value is added after two parts solution blending to 5.5,85 DEG C of reaction 3h；
(2) it is added magnesium hydroxide again, adjusts pH value to 8.5, acetaldehyde is then added and (urea and acetaldehyde are added in step (1)
The mass ratio of the material is 1:0.8), 75 DEG C of reaction 4h obtain the modified urea-formaldehyde solution that aldehyde is 0.08%；
(3) gained spinning solution is by wet spinning, use saturated aqueous sodium sulfate that weight content is 1.9% boric acid as
Coagulating bath, winding speed is that 50m/min obtains as-spun fibre at 40 DEG C of temperature, then after 30 DEG C of drying, is heated up with 20 DEG C/min
It 190 DEG C, constant temperature 1h, takes out after Temperature fall up to ureaformaldehyde fiber.
The ureaformaldehyde fibre diameter of preparation is 21 microns, tensile strength 390MPa, elongation at break 29%, the LOI of fiber
Value is 32.
Embodiment 8
The preparation method of the melamine modified urea-formaldehyde fiber of the present embodiment, steps are as follows:
(1) by the PVA PVA aqueous solution soluble in water for obtaining 8wt%, two parts are divided into, melamine, acetaldehyde is added in a part
And potassium hydroxide, 3.8h is reacted under the conditions of pH is 7.8,60 DEG C, and the molar ratio of melamine and acetaldehyde is 1:0.9, wherein PVA
The mass ratio of melamine is 1:0.9；Urea and formaldehyde (molar ratio 1:1.2) is added in another part, wherein PVA and urea
Mass ratio be 1:3.6:0.9；Then sodium hydroxide is added, adjusts pH value to 8.5, in 90 DEG C of reaction 2h；Two parts solution is total
Salt acid for adjusting pH value is added after mixed to 5.5,85 DEG C of reaction 3h；
(2) it is added sodium hydroxide again, adjusts pH value to 8.5, formaldehyde is then added and (urea and formaldehyde are added in step (1)
The mass ratio of the material is 1:0.8), 75 DEG C of reaction 2h obtain the modified urea-formaldehyde solution that aldehyde is 0.11%；
(3) gained spinning solution is by wet spinning, uses saturated aqueous sodium sulfate that weight content is 2% boric acid as coagulating
Gu bathing, winding speed is that 20m/min obtains as-spun fibre at 40 DEG C of temperature, then after 30 DEG C of dryings, with 20 DEG C/min heating 190
DEG C, constant temperature 1.5h takes out after Temperature fall up to ureaformaldehyde fiber.
The ureaformaldehyde fibre diameter of preparation is 28 microns, tensile strength 380MPa, elongation at break 31%, the LOI of fiber
Value is 33.
Basic principles and main features and advantages of the present invention of the invention have been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (9)
1. a kind of preparation method of melamine modified urea-formaldehyde fiber, which is characterized in that its steps is as follows:
(1) water soluble polymer aqueous solution is obtained by water soluble polymer is soluble in water, by water soluble polymer aqueous solution equal part
At A, B two parts, melamine, aldehydes and basic catalyst are added into part A solution, is reacted under the conditions of 50-95 DEG C
0.4-10h obtains first solution；Urea and aldehyde compound and basic catalyst are added into part B solution, then in 45-
0.5-8h is reacted under the conditions of 95 DEG C, obtains second solution；PH value is adjusted after the mixing of first, second solution to acidity, under the conditions of 40-95 DEG C
The reaction was continued 0.1-7h, obtains modified urea-formaldehyde resin solution；
(2) basic catalyst is added and adjusts modified urea-formaldehyde resin solution to alkalinity, and is slowly added to aldehyde compound, in 35-95
After reacting a period of time under the conditions of DEG C, modified urea-formaldehyde spinning solution is obtained, using wet spinning technology, is obtained after coagulating bath
Ureaformaldehyde as-spun fibre；
(3) then as-spun fibre is heating and curing in an oven according to certain heating rate, obtains by washing, drying
Modified urea-formaldehyde fiber.
2. the preparation method of the melamine modified urea-formaldehyde fiber according to claim 1, it is characterised in that: the step
(1) water soluble polymer is PVA, PEG, polyvinyl formal, PVP, water-soluble modified starch or water-soluble modified fiber in
One of element；High molecular mass content is 1-30% in water soluble polymer aqueous solution.
3. the preparation method of the melamine modified urea-formaldehyde fiber according to claim 1, it is characterised in that: the aldehydes
Compound is one of formaldehyde, glutaraldehyde, acetaldehyde, paraformaldehyde；Basic catalyst is sodium hydroxide, potassium hydroxide, three second
One of hydramine, sodium bicarbonate, magnesium hydroxide or calcium hydroxide, acidic catalyst are in hydrochloric acid, sulfuric acid, phosphoric acid or oxalic acid
It is a kind of.
4. the preparation method of the melamine modified urea-formaldehyde fiber according to claim 1, it is characterised in that: the step
(1) in part A solution, the molar ratio of melamine and aldehydes is 1:(0.7-1.9), the mass ratio of macromolecule and melamine is
1:(0.1-4)；The molar ratio of urea and aldehydes is 1:(0.7-1.9 in part B solution), the mass ratio of macromolecule and urea is 1:
(0.2-10).
5. the preparation method of the melamine modified urea-formaldehyde fiber according to claim 1, it is characterised in that: the step
(1) pH value range of first solution is 7.4-11 in, and the pH value range of second solution is 7.5-10.5, is adjusted after the mixing of first, second solution
PH value range is 4.0-6.9.
6. the preparation method of the melamine modified urea-formaldehyde fiber according to claim 1, it is characterised in that: the step
(2) it is 7.4-10.5, reaction time 0.4-8h that basic catalyst is added in and adjusts urea-formaldehyde resin solution pH value range.
7. the preparation method of the melamine modified urea-formaldehyde fiber according to claim 1, it is characterised in that: the step
(2) for the additional amount of aldehyde compound on the basis of urea in step (1), the mass ratio of the material of urea and aldehyde compound is 1:
(0.3-2).
8. the preparation method of the melamine modified urea-formaldehyde fiber according to claim 1, it is characterised in that: the step
(2) coagulating bath of wet spinning is saturated aqueous sodium sulfate in, and adds the boric acid that weight content is 0.1-5%, and temperature is
10-60 DEG C, winding speed 10-500m/min.
9. the preparation method of the melamine modified urea-formaldehyde fiber according to claim 1, it is characterised in that: the step
(3) for as-spun fibre at 20-40 DEG C of drying temperature of vacuum drying oven, heating rate is 1-30 DEG C/min in, is warming up to 150-230
DEG C, constant temperature 0.1-2h takes out after Temperature fall up to modified urea-formaldehyde fiber.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN110820074A (en) * | 2019-11-27 | 2020-02-21 | 中原工学院 | Method for preparing urea compound modified melamine fiber by base catalysis |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110714234A (en) * | 2019-11-27 | 2020-01-21 | 中原工学院 | Method for preparing urea compound modified melamine fiber by copolymerization |
| CN110820074A (en) * | 2019-11-27 | 2020-02-21 | 中原工学院 | Method for preparing urea compound modified melamine fiber by base catalysis |
| CN110846740A (en) * | 2019-11-27 | 2020-02-28 | 中原工学院 | Method for preparing phenol modified melamine fiber by single-kettle method |
| CN110846737A (en) * | 2019-11-27 | 2020-02-28 | 中原工学院 | Method for preparing phenolic modified melamine fiber by one-step method |
| CN110846740B (en) * | 2019-11-27 | 2022-07-15 | 中原工学院 | Method for preparing phenol modified melamine fiber by single-kettle method |
| CN117050440A (en) * | 2023-09-07 | 2023-11-14 | 揭阳市顺佳和化工有限公司 | Modified amino molding compound and preparation method thereof |
| CN117050440B (en) * | 2023-09-07 | 2024-02-06 | 揭阳市顺佳和化工有限公司 | Modified amino molding compound and preparation method thereof |
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