CN104927066B - Dye dispersant and preparation method thereof - Google Patents
Dye dispersant and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of preparation method of dye dispersant, including：Lignocellulosic boiling in the presence of catalyst, obtains cellulose and black liquor；The catalyst is methylol sulfonate；Black Liquor Concentration obtains dye dispersant.Not only staining performance is good but also heat-resistant stability is good for the dye dispersant that the present invention is obtained by the boiling lignocellulosic in the presence of specific catalyst.Test result indicate that：The dye dispersant diffusion that preparation method of the present invention is prepared is 5 grades of normal temperature；Heat-resistant stability is 120 DEG C, more than 5 grades；Cotton stains performance and is more than 4 grades；Terylene stains performance and is more than 3 grades；40% solid content viscosity is 20~1000mp.s.
Description
Technical field
The present invention relates to technical field of biochemical industry, more particularly, to a kind of dye dispersant and preparation method thereof.
Background technology
Dye composite is widely used in the dyeing of natural and synthetic fibers, generally comprises dyestuff block and dispersant, disperses
The effect of agent can help to reduce the particle diameter of dye granule primarily as diluent, energy decentralized medium.
Lignosulfonates are a kind of conventional dye dispersants, are net macromolecular structure, and its source mainly has：1) come
The lignosulfonate (through sulfurous acid pulp-making method or sulfate (kraft) pulp-making method) of wood pulping industry is come from, specifically, passing through
Lignocellulosic materials (such as timber, straw, cornstalk, bagasse and the like) are processed, makes lignin and cellulose
Or paper pulp is separated, and obtains lignosulfonate；2) from the naphthalene sulfonate of petroleum industry.Lignosulfonates are used as dye set
The advantage of the dispersant of compound has：Raw material sources extensively, and under room temperature and high temperature with many dyestuffs have well it is compatible
Property and dispersive property.
In the prior art by the dye dispersant of the preparation such as lignin black liquor not only staining poor performance, and Heat-resistant stable
Property is poor.
The content of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of preparation method of dye dispersant, this hair
Dye dispersant staining performance that the method for the preparation of the dye dispersant of bright offer is prepared is good, heat-resistant stability is good.
The invention provides a kind of preparation method of dye dispersant, including：
Lignocellulosic boiling in the presence of catalyst, obtains cellulose and black liquor；The catalyst is methylol sulphur
Hydrochlorate；
Black Liquor Concentration obtains dye dispersant.
Preferably, the mole (mmol) of the catalyst accounts for the quality (g) of the lignocellulosic than being 0.1:1~4:
1。
Preferably, the boiling pH value is 6~12.
Preferably, the cooking reaction liquid-solid ratio is 2~20:1.
Preferably, the catalyst be sodium hydroxymethane sulfonate, methylol potassium sulfonate and methylol sulfonic acid magnesium in one kind or
It is several.
Preferably, the temperature of the boiling is 90~165 DEG C.
Preferably, solid content is 20%~60% after the concentration.
Preferably, the lignocellulosic is prepared in accordance with the following methods：
The acidolysis in the presence of catalyst of lignin raw material, obtains lignocellulosic；The catalyst includes non-oxidizable
Acid and sulphite；The non-oxidizing acid includes the first non-oxidizing acid and the second non-oxidizing acid；Described first is non-oxide
Property acid be sulfurous acid.
The invention provides a kind of dye dispersant, prepared by the preparation method of the claims any one.
Compared with prior art, the invention provides a kind of preparation method of dye dispersant, including：Lignocellulosic exists
Boiling in the presence of catalyst, obtains cellulose and black liquor；The catalyst is methylol sulfonate；Black Liquor Concentration obtains dyestuff
Dispersant.The dye dispersant not only staining that the present invention is obtained by the boiling lignocellulosic in the presence of specific catalyst
Performance is good and heat-resistant stability is good.Test result indicate that：The dye dispersant diffusivity that preparation method of the present invention is prepared
Can be 5 grades of normal temperature；Heat-resistant stability is 130 DEG C, more than 5 grades；Cotton stains performance and is more than 4 grades；Terylene stains performance and is more than 3
Level；40% solid content viscosity is 20~1000mp.s.
Specific embodiment
The invention provides a kind of preparation method of dye dispersant, including：
Lignocellulosic boiling in the presence of catalyst, obtains cellulose and black liquor；The catalyst is methylol sulphur
Hydrochlorate；
Black Liquor Concentration obtains dye dispersant.
The present invention is not defined for the source of the lignocellulosic, can be conventional xylose residue or furfural dregs.
It is preferred that being prepared using following methods：
The acidolysis in the presence of catalyst of lignin raw material, obtains lignocellulosic；The catalyst includes non-oxidizable
Acid and sulphite；The non-oxidizing acid includes the first non-oxidizing acid and the second non-oxidizing acid；Described first is non-oxide
Property acid be sulfurous acid.
In the present invention, lignin raw material acidolysis in the presence of catalyst first, obtains liquid glucose.The present invention is for described
Lignin raw material be not defined, be preferably selected from one or more in corncob, reed, beans bar and cotton stalk；More preferably
Corncob or reed；Most preferably corncob.Raw material of the invention preferably through crushing, the present invention for crushing instrument or
The mesh number that crushing is obtained is not defined, instrument and mesh number that acidolysis well known to those skilled in the art is crushed.
Catalyst of the present invention includes non-oxidizing acid and sulphite；The non-oxidizing acid includes that first is non-oxide
Property acid and the second non-oxidizing acid；First non-oxidizing acid is sulfurous acid.Second non-oxidizing acid is preferably selected from phosphorus
One or more in acid, sulfuric acid, oxalic acid and acetic acid；Second non-oxidizing acid be more preferably selected from phosphoric acid, sulfuric acid, oxalic acid and
Two or more in acetic acid；The sulphite is preferably selected from potassium sulfite, sodium sulfite, magnesium sulfite and sulfurous acid
One or more in calcium.
In the present invention, the non-oxidizing acid is preferably (1~10) with the mass ratio of lignin raw material：100, more preferably
It is (3~8)：100, most preferably (3~6)：100.The mass ratio of first non-oxidizing acid and the second non-oxidizing acid is excellent
Elect as (1~99)：(1~99), more preferably (50~99)：(1~50), most preferably (50~99)：(1~50), most preferably
It is (70~90)：(5~30)；The mol ratio of the sulphite and the first non-oxidizing acid is preferably (1~10)：100, it is more excellent
Elect as (2~7)：100, most preferably (3~4.5)：100.The solid-to-liquid ratio of the acidolysis reaction is preferably greater than 2:1；It is more preferably big
In 4:1；Most preferably greater than 5.5:1.The temperature of the acidolysis is preferably 110~160 DEG C, more preferably 120~150 DEG C, optimal
Elect 125~140 DEG C as.The pressure of the acidolysis is preferably 0.2~0.7MPa, more preferably 0.4~0.7MPa, most preferably
0.5~0.7MPa.
The acidolysis finish after preferably through separation of solid and liquid, obtain liquid glucose and sugar residue, the liquid glucose can be used for preparing
Furfural or xylose, the sugar residue are washed preferably through first time, and the temperature of the first time washing is preferably 90~130 DEG C, more
Preferably 90~120 DEG C, most preferably 90~100 DEG C.The liquid-solid ratio of the washing is preferably 2:1~6:1, more preferably 4：1
~6:1, most preferably 6:1~8:1；Separation of solid and liquid after washing, obtains liquid glucose and sugar residue, and liquid glucose is merged；Sugar residue is carried out
Secondary washing, the temperature of second washing is preferably 70~110 DEG C, more preferably 70~100 DEG C, most preferably 70~90
℃.The liquid-solid ratio of the washing is preferably 2:1~6:1, more preferably 4：1~6:1, most preferably 6:1~8:1；It is solid after washing
Liquid is separated, and obtains liquid glucose and lignocellulosic.
The index of the lignocellulosic that the present invention is obtained preferably can be：
The weight/mass percentage composition of the cellulose is preferably 60%~70%, more preferably 63%~68%, most preferably
64%~67%；The weight/mass percentage composition of the hemicellulose is preferably 0%~10%, more preferably 1%~8%, most preferably
It is 3%~7%；The weight/mass percentage composition of the lignin is preferably 20%~30%, more preferably 22%~28%, most preferably
It is 24%~27%；The ash content is preferably less than 5 percent, more preferably less than 3 percent, most preferably less than percentage
Two.
In the present invention, lignocellulosic boiling in the presence of catalyst, obtains cellulose and black liquor.The catalyst
It is methylol sulfonate；The catalyst is preferably in sodium hydroxymethane sulfonate, methylol potassium sulfonate and methylol sulfonic acid magnesium
Plant or several.In the present invention, the catalyst is preferably prepared in accordance with the following methods：With formaldehyde and bisulfites or sulfurous acid
Salt or sulfur dioxide addition are obtained；The bisulfites can be selected from sodium hydrogensulfite, potassium bisulfite etc.；Sulphite is
Sodium sulfite, potassium sulfite etc..
In the present invention, the catalyst accounts for the mass percent of the lignocellulosic and is preferably 2%~20%, more excellent
Elect 4%~15%, most preferably 6%~10% as.
In the present invention, the pH value of the cooking reaction is preferably 6~12, more preferably 6~11, most preferably 7~11.
The liquid-solid ratio of the boiling is preferably 2~20:1, more preferably (2~15):1, most preferably (2~10):1；The boiling
Temperature is preferably 90~165 DEG C, more preferably 90~140 DEG C.The present invention is not particularly limited to the container for reacting, and this area is public
The container known, as digester, rotary spherical digester or reactor；The present invention is not also special to the mode of heating for reacting
Limitation, directly heats or indirectly heat.
By black liquor by separation of solid and liquid, solid and liquid are obtained；Solid for the first time wash after separation of solid and liquid obtain solid and
Liquid；The temperature of the first time washing is preferably 30~80 DEG C, most preferably more preferably 30~60 DEG C, 30~50 DEG C；Institute
The slurry mass concentration for stating washing for the first time is preferably 2%~10%, more preferably 4%~8%, most preferably 4%~6%；The
Once wash the solid for obtaining and obtain crude fibre and black liquor by second washing separation of solid and liquid；The temperature of second washing
Degree is preferably 30~80 DEG C, most preferably more preferably 30~60 DEG C, 30~50 DEG C；The slurry concentration of second washing is preferred
It is 2%~10%, more preferably 4%~8%, most preferably 4%~6%.
The present invention is not defined for the equipment used by the separation of solid and liquid, sheet frame well known to those skilled in the art,
Any one in squeezer, twin-wire press.
The liquid that above-mentioned separation of solid and liquid is obtained can be used for adverse current set and wash, and the liquid for finally obtaining merges, for preparing wood
Mahogany sulfonate.
Above-mentioned isolated liquid is concentrated after merging, and solid content is preferably 20%~60% after present invention concentration, more excellent
Elect 20%~40% as.
After concentration lignosulfonates are obtained preferably through spray drying.Equipment for the spray drying of the invention is not
It is defined, equipment well known to those skilled in the art.The EAT is preferably 220~280 DEG C, more preferably
240~280 DEG C, most preferably 260~280 DEG C；The leaving air temp is preferably 90~130 DEG C, more preferably 90~120 DEG C,
Most preferably 90~110 DEG C.
The product index of the lignosulfonates that sugar residue is obtained is：1% pH value of water solution is 9~10, and reduced sugar accounts for described
The weight/mass percentage composition of dry be less than or equal to 4%, the weight/mass percentage composition that water-insoluble accounts for the dry be less than etc.
In 0.03%, sulfate weight/mass percentage composition is 2%~6%, and sulfonation degree is 0.7~0.9, preferably 0.8.
The invention provides a kind of dye dispersant, prepared by above-mentioned preparation method.
The invention provides a kind of preparation method of dye dispersant, including：Lignocellulosic is in the presence of catalyst
Boiling, obtains cellulose and black liquor；The catalyst is methylol sulfonate；Black Liquor Concentration obtains dye dispersant.The present invention
Not only staining performance is good for the dye dispersant obtained by the boiling lignocellulosic in the presence of specific catalyst, Er Qienai
Heat endurance is good.
In order to further illustrate the present invention, the preparation method of the dye dispersant for providing the present invention with reference to embodiments
It is described in detail.
Embodiment 1
100g corncobs are crushed, and add 5g sulfurous acid, 5g phosphoric acid, 0.6g sodium sulfites to be hydrolyzed under 110 DEG C, 0.4Mpa,
Obtain liquid glucose；After separation of solid and liquid, liquid glucose and sugar residue are obtained；Merge liquid glucose, sugar residue adds four times of 100 DEG C of washings, separation of solid and liquid
Afterwards, liquid glucose and sugar residue are obtained；Merge liquid glucose, sugar residue adds 100 DEG C of washings of twice, 55g wood fibres are obtained after separation of solid and liquid
Element, after testing lignocellulosic index be：The weight/mass percentage composition of cellulose is 65%；The weight/mass percentage composition of hemicellulose is
7%；The weight/mass percentage composition of lignin is 26%；Ash content is 2%.
Take 55g lignocellulosics, add 6g sodium hydroxymethane sulfonates, regulation pH value is 6,90 DEG C of reactions, obtain cellulose and
Black liquor, black liquor separation of solid and liquid obtains solid-liquid and liquid, and solid is washed under conditions of 30 DEG C, slurry mass concentration are for 4%；Solid
Separation of solid and liquid, 40 DEG C of washings again, separation of solid and liquid, merging obtains liquid, is 20% by liquid concentration to solid content, then sprays
Dry, spray drying EAT is 220 DEG C, and leaving air temp is 90 DEG C, obtains dye dispersant.After testing, wherein sulfate
Content is 5%, and total reduzate content is 3%, and sulfonation degree is 0.7, and 1% pH value of water solution is 9.
Detection method according to HG/T3507-2008 is examined to the staining performance and heat-resistant stability of dye dispersant
Survey, as a result show, it is 3~4 grades that its cotton stains, it is 3 grades that terylene stains；Heat resistance is 150 DEG C 5 grades；Diffusion is normal
5 grades of temperature.
Embodiment 2
200g corncobs are crushed, and add 13g sulfurous acid, 3g oxalic acid, 1.1g sodium sulfites to be hydrolyzed under 160 DEG C, 0.5Mpa,
Obtain liquid glucose；After separation of solid and liquid, liquid glucose and sugar residue are obtained；Merge liquid glucose, sugar residue adds six times of 100 DEG C of washings, separation of solid and liquid
Afterwards, liquid glucose and sugar residue are obtained；Merge liquid glucose, sugar residue adds four times of 90 DEG C of washings, 110g wood fibres are obtained after separation of solid and liquid
Element, after testing lignocellulosic index be：The weight/mass percentage composition of cellulose is 65%；The weight/mass percentage composition of hemicellulose is
7%；The weight/mass percentage composition of lignin is 26%；Ash content is 2%.
110g lignocellulosics are taken, 13g sodium hydroxymethane sulfonates are added, regulation pH value is 7,110 DEG C of reactions, obtains cellulose
And black liquor, black liquor separation of solid and liquid obtains solid-liquid and liquid, solid 50 DEG C, slurry mass concentration be 6% under conditions of wash；Gu
Body separation of solid and liquid, 50 DEG C of washings again, separation of solid and liquid, merging obtains liquid, is 30% by liquid concentration to solid content, then sprays
Mist is dried, and spray drying EAT is 220 DEG C, and leaving air temp is 90 DEG C, obtains dye dispersant.After testing, wherein sulfuric acid
Salt content is 5%, and total reduzate content is 3%, and sulfonation degree is 0.8, and 1% pH value of water solution is 9.
Detection method according to HG/T3507-2008 is examined to the staining performance and heat-resistant stability of dye dispersant
Survey, as a result show, it is 3~4 grades that its cotton stains, it is 3 grades that terylene stains；Heat resistance is 150 DEG C 5 grades；Diffusion is normal
5 grades of temperature.
Embodiment 3
300g corncobs are crushed, and add 10g sulfurous acid, 5g sulfuric acid, 1.3g sodium sulfites to be hydrolyzed under 150 DEG C, 0.6Mpa,
Obtain liquid glucose；After separation of solid and liquid, liquid glucose and sugar residue are obtained；Merge liquid glucose, sugar residue adds four times of 100 DEG C of washings, separation of solid and liquid
After obtain 165g lignocellulosics, lignocellulosic index is after testing：The weight/mass percentage composition of cellulose is 65%；Half fiber
The weight/mass percentage composition of element is 7%；The weight/mass percentage composition of lignin is 26%；Ash content is 2%.
165g lignocellulosics are taken, 22g methylol potassium sulfonates are added, regulation pH value is 11,140 DEG C of reactions, obtains fiber
Element and black liquor, black liquor separation of solid and liquid obtain solid-liquid and liquid, and solid is washed under conditions of 50 DEG C, slurry mass concentration are for 6%；
Solid separation of solid and liquid again, 60 DEG C of washings, separation of solid and liquid, merging obtains liquid, is 40% by liquid concentration to solid content, then
Spray drying, spray drying EAT is 220 DEG C, and leaving air temp is 90 DEG C, obtains dye dispersant.After testing, wherein sulphur
Phosphate content is 5%, and total reduzate content is 3%, and sulfonation degree is 0.9, and 1% pH value of water solution is 10.
Detection method according to HG/T3507-2008 is examined to the staining performance and heat-resistant stability of dye dispersant
Survey, as a result show, it is 3~4 grades that its cotton stains, it is 3 grades that terylene stains；Heat resistance is 150 DEG C 5 grades；Diffusion is normal
5 grades of temperature.
Embodiment 4
300g corncobs are crushed, and add 10g sulfurous acid, 5g acetic acid, 1.3g sodium sulfites to be hydrolyzed under 150 DEG C, 0.6Mpa,
Obtain liquid glucose；After separation of solid and liquid, liquid glucose and sugar residue are obtained；Merge liquid glucose, sugar residue adds four times of 100 DEG C of washings, separation of solid and liquid
After obtain 165g lignocellulosics, lignocellulosic index is after testing：The weight/mass percentage composition of cellulose is 65%；Half fiber
The weight/mass percentage composition of element is 7%；The weight/mass percentage composition of lignin is 26%；Ash content is 2%.
165g lignocellulosics are taken, 25g sodium hydroxymethane sulfonates are added, regulation pH value is 11,150 DEG C of reactions, obtains fiber
Element and black liquor, black liquor separation of solid and liquid obtain solid-liquid and liquid, and solid is washed under conditions of 30 DEG C, slurry mass concentration are for 4%；
Solid separation of solid and liquid again, 40 DEG C of washings, separation of solid and liquid, merging obtains liquid, is 50% by liquid concentration to solid content, then
Spray drying, spray drying EAT is 220 DEG C, and leaving air temp is 90 DEG C, obtains dye dispersant.After testing, wherein sulphur
Phosphate content is 5%, and total reduzate content is 3%, and sulfonation degree is 1.0, and 1% pH value of water solution is 10.
Detection method according to HG/T3507-2008 is examined to the staining performance and heat-resistant stability of dye dispersant
Survey, as a result show, it is 3~4 grades that its cotton stains, it is 3 grades that terylene stains；Heat resistance is 150 DEG C 5 grades；Diffusion is normal
5 grades of temperature.
Embodiment 5
300g corncobs are crushed, and add 10g sulfurous acid, 2g acetic acid, 3g sulfuric acid, 1.3g sodium sulfites in 150 DEG C, 0.6Mpa
Lower hydrolysis, obtains liquid glucose；After separation of solid and liquid, liquid glucose and sugar residue are obtained；Merge liquid glucose, sugar residue adds four times of 100 DEG C of washings, Gu
After liquid is separated, 165g lignocellulosics are obtained, lignocellulosic index is after testing：The weight/mass percentage composition of cellulose is
65%；The weight/mass percentage composition of hemicellulose is 7%；The weight/mass percentage composition of lignin is 26%；Ash content is 2%.
Formaldehyde is obtained sodium hydroxymethane sulfonate with sodium hydrogensulfite in 60~65 DEG C of additions.
165g lignocellulosics are taken, the above-mentioned 19g sodium hydroxymethane sulfonates for preparing are added, regulation pH value is 10,120 DEG C
Reaction, obtains cellulose and black liquor, and black liquor separation of solid and liquid obtains solid-liquid and liquid, and solid is 4% in 40 DEG C, slurry mass concentration
Under conditions of wash；Solid separation of solid and liquid again, 50 DEG C of washings, separation of solid and liquid, merging obtains liquid, by liquid concentration to containing admittedly
It is 40% to measure, and is then spray-dried, and spray drying EAT is 220 DEG C, and leaving air temp is 90 DEG C, obtains dye dispersant.
After testing, wherein sulphates content is 5%, and total reduzate content is 3%, and sulfonation degree is 0.8, and 1% pH value of water solution is 9.
Detection method according to HG/T3507-2008 is examined to the staining performance and heat-resistant stability of dye dispersant
Survey, as a result show, it is 3~4 grades that its cotton stains, it is 3 grades that terylene stains；Heat resistance is 150 DEG C 5 grades；Diffusion is normal
5 grades of temperature.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of preparation method of dye dispersant, including：
Lignocellulosic boiling in the presence of catalyst, obtains cellulose and black liquor；The catalyst is methylol sulfonate；
The lignocellulosic is prepared in accordance with the following methods：
The acidolysis in the presence of catalyst of lignin raw material, obtains lignocellulosic；The catalyst include non-oxidizing acid and
Sulphite；The non-oxidizing acid includes the first non-oxidizing acid and the second non-oxidizing acid；First non-oxidizing acid
It is sulfurous acid；Second non-oxidizing acid is selected from one or more in phosphoric acid, sulfuric acid, oxalic acid and acetic acid；
Black Liquor Concentration obtains dye dispersant.
2. preparation method according to claim 1, it is characterised in that the catalyst accounts for the quality of the lignocellulosic
Percentage is 2%~20%.
3. preparation method according to claim 1, it is characterised in that the boiling pH value is 6~12.
4. preparation method according to claim 1, it is characterised in that the cooking reaction liquid-solid ratio is 2~20:1.
5. preparation method according to claim 1, it is characterised in that the catalyst is sodium hydroxymethane sulfonate, methylol
One or more in potassium sulfonate and methylol sulfonic acid magnesium.
6. preparation method according to claim 1, it is characterised in that the temperature of the boiling is 90~165 DEG C.
7. preparation method according to claim 1, it is characterised in that solid content is 20%~60% after the concentration.
8. a kind of dye dispersant, is prepared by the preparation method of claim 1~7 any one.
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