CN109338482A - A kind of preparation method of nanocomposite degumming and refining agent - Google Patents
A kind of preparation method of nanocomposite degumming and refining agent Download PDFInfo
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- CN109338482A CN109338482A CN201811106564.8A CN201811106564A CN109338482A CN 109338482 A CN109338482 A CN 109338482A CN 201811106564 A CN201811106564 A CN 201811106564A CN 109338482 A CN109338482 A CN 109338482A
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- degumming
- nanocomposite
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01C—CHEMICAL OR BIOLOGICAL TREATMENT OF NATURAL FILAMENTARY OR FIBROUS MATERIAL TO OBTAIN FILAMENTS OR FIBRES FOR SPINNING; CARBONISING RAGS TO RECOVER ANIMAL FIBRES
- D01C3/00—Treatment of animal material, e.g. chemical scouring of wool
- D01C3/02—De-gumming silk
Abstract
The present invention provides a kind of preparation methods of nanocomposite degumming and refining agent, the nanocomposite degumming catalyst is prepared by the raw material of following weight percent: nano-titanium dioxide 1-10%, nano silica 0.5-5%, sodium carbonate 10-40%, rare earth 0.1-10%, anthraquinone analog compound 1-10%, remaining is water.Preparation method, which includes: (1), is mixed to prepare A liquid for nano-titanium dioxide and water；(2) nano silica and water are mixed to prepare B liquid；(3) A liquid and B liquid are mixed to prepare nanocomposite；(4) rare earth and water are mixed to prepare C liquid；(5) nanocomposite and C liquid are mixed to prepare D liquid；(6) sodium carbonate is added in D liquid, adjusting pH is 10-13, and degumming catalyst is made after agitated, mixing, ultrasonic treatment.The degumming catalyst has good degumming effect, and the silk fabric after degumming still keeps good mechanical strength.
Description
Technical field
The invention belongs to degumming tech technical fields, and in particular to a kind of preparation side of nanocomposite degumming and refining agent
Method.
Background technique
Silk obtains people with the feel of the wearability of its comfort health-care, the appearance of elegant pendency and smooth pliable
Favor, be known as " fiber queen ".In silk raw material in addition to main component fibroin, also containing a considerable amount of silk gum and less
Measure the sundries such as grease, wax, hair, grass cuttings.Wherein silk gum has certain protective effect, silk gum in general silk fiber to fibroin
Account for about 1/4 or so.Content of silk gum is excessive, then will affect fibroin gloss and feel and the technique of silk fiber processing, grease, wax
The impurity such as matter can bring certain difficulty to post-processing.Therefore, natural silk degumming is an important process ring for influencing silk quality
Section needs to carry out strict control to degumming tech condition, could obtain stable high-quality silk product.
The Degumming method of silk mainly uses chemical method and microbial method at present, however obtained after both methods degumming
Silk fiber, soft smooth, high resilience, good luster, but usually time is long, and the easy yellowing of white fabrics after degumming,
It is larger to the damage of silk after chemical degumming.Continuous promotion with people to product quality requirement, it is necessary to which silk is knitted
The degumming tech of object is further studied, and novel degumming product is developed, to improve the quality of silk product.
Summary of the invention
Above of the existing technology in order to solve the problems, such as, it is de- that the purpose of the present invention is to provide a kind of nanocomposites
The preparation method of glue refining agent.
To achieve the goals above, the present invention the following technical schemes are provided:
A kind of nanocomposite degumming and refining agent, the nanocomposite degumming catalyst is by following weight percent
Raw material is prepared: nano-titanium dioxide 1-10%, nano silica 0.5-5%, sodium carbonate 10-40%, rare earth 0.1-10%, anthracene
Quinones 1-10%, remaining is water.
Preferably, a kind of nanocomposite degumming and refining agent of the present invention, the nanocomposite degumming
Catalyst is prepared by the raw material of following weight percent: nano-titanium dioxide 5%, nano silica 3%, sodium carbonate 25%,
Rare earth 5%, anthraquinone analog compound 5%, remaining is water.
Preferably, a kind of nanocomposite degumming and refining agent of the present invention, the nano-titanium dioxide are grain
Diameter is 50-80nm, and nano silica partial size is 40-70nm, and sodium carbonate is light sodium carbonate, and rare earth is ion adsorption type re
(mischmetal containing REO > 60% is to form the clay mineralizer containing rare earth through many years weathering, in strong electrolyte such as NaCl, (NH4)2SO4、NH4Ion exchange can occur in the alkaline solutions such as Cl and enter solution and there is reversible reaction), anthraquinone compounds are free
Anthraquinone.
Further, a kind of nanocomposite degumming and refining agent of the present invention, the dissociated anthraquinone are rheum officinale
One or more combinations of phenol, rheum emodin, Physcion, aloe-emodin or Rhein.
A kind of preparation method of nanocomposite degumming and refining agent of the present invention, comprising the following steps:
(1) the dedicated high shear dispersion machine of nano material is used, adjustment revolution is 5000-10000 revs/min, by nano-silica
Change and carry out high speed shear dispersion 5-30min after titanium is mixed with the one third of water inventory, discharges and A liquid is made；
(2) the dedicated high shear dispersion machine of nano material is used, adjustment revolution is 5000-10000 revs/min, takes proper amount of nano
Silica carries out high speed shear dispersion 5-30min after mixing with the one third of water inventory, discharge and B liquid is made；
(3) A liquid and B liquid are uniformly mixed under agitation, obtain nanocomposite, discharged spare；
(4) after mixing rare earth with the one third of water inventory, anthraquinone analog compound is added under stirring conditions, rotates forward stirring
10-30min, then stirring 5-10min discharging is inverted, C liquid is made；
(5) nanocomposite and C liquid are subjected to homogeneous under agitation, D liquid is made after mixing evenly；
(6) sodium carbonate is added into D liquid under agitation, adjusting pH is 10-13, under stirring conditions by solution temperature liter
Up to 45-60 DEG C, after being stirred to react 20-50min, supernatant is removed by centrifugation, lower sediment particle is made by ultrasound
Precipitating particle is uniformly dispersed, and the discharging of 0.2-0.3mm powder particle, as the nanocomposite degumming catalyst is made.
A kind of application of the nanocomposite degumming and refining agent of the present invention in degumming tech.
The utility model has the advantages that the present invention provides a kind of nanocomposite degumming and refining agent Preparation method and use, the present invention
Degumming catalyst, nanocomposite pair produced by the present invention are mixed with by nano material and rare earth, anthraquinone analog compound
Silk fabric has good degumming effect, while nanofiller plays crucial effect to the degumming of silk fabric, and makes
After carrying out degumming with the nanocomposite, silk fabric still maintains good mechanical strength, not to the mechanical property of fabric
Destructive influences can be generated, and add the nanocomposite of anthraquinone analog compound and rare earth to after silk fabric processing with
Un-added, color more brilliant white more preferable compared to degumming effect mentions to illustrate that the compounding of anthraquinone analog compound and rare earth plays
High retting function, the effect for improving bleaching effect.Therefore nanocomposite degumming catalyst produced by the present invention is in degumming work
It is with a wide range of applications in skill.
Specific embodiment
The invention will now be further described with reference to specific embodiments, but examples are merely exemplary, not to this hair
Bright range constitutes any restrictions.It will be understood by those skilled in the art that without departing from the spirit and scope of the invention
Can with the details and forms of the technical scheme of the invention are modified or replaced, but these modification and replacement each fall within it is of the invention
In protection scope.
Embodiment 1
A kind of nanocomposite degumming and refining agent, the nanocomposite degumming catalyst is by following weight percent
Raw material is prepared: nano-titanium dioxide 5%, nano silica 3%, sodium carbonate 25%, rare earth 5%, anthraquinone analog compound 5%,
Yu Weishui.
The nano-titanium dioxide is that partial size is 65nm, and nano silica partial size is 55nm, and sodium carbonate is lightweight carbon
Sour sodium, rare earth are ion adsorption type re, and anthraquinone compounds are dissociated anthraquinone, and the dissociated anthraquinone is that mass ratio is 1:1's
Chrysophanol and rheum emodin.
A kind of preparation method of nanocomposite degumming and refining agent of the present invention, comprising the following steps:
(1) use the dedicated high shear dispersion machine of nano material, adjustment revolution be 8000 revs/min, by nano-titanium dioxide with
High speed shear is carried out after the one third mixing of water inventory and disperses 18min, discharges and A liquid is made；
(2) the dedicated high shear dispersion machine of nano material is used, adjustment revolution is 8000 revs/min, takes proper amount of nano titanium dioxide
Silicon carries out high speed shear dispersion 20min after mixing with the one third of water inventory, discharge and B liquid is made；
(3) A liquid and B liquid are uniformly mixed under agitation, obtain nanocomposite, discharged spare；
(4) after mixing rare earth with the one third of water inventory, anthraquinone analog compound is added under stirring conditions, rotates forward stirring
20min, then stirring 8min discharging is inverted, C liquid is made；
(5) nanocomposite and C liquid are subjected to homogeneous under agitation, D liquid is made after mixing evenly；
(6) sodium carbonate is added into D liquid under agitation, adjusting pH is 10-13, under stirring conditions by solution temperature liter
Up to 53 DEG C, after being stirred to react 35min, supernatant is removed by centrifugation, lower sediment particle is made into precipitating by ultrasound
Grain is uniformly dispersed, and the discharging of 0.2-0.3mm powder particle, as the nanocomposite degumming catalyst is made.
Embodiment 2
A kind of nanocomposite degumming and refining agent, the nanocomposite degumming catalyst is by following weight percent
Raw material is prepared: nano-titanium dioxide 1%, nano silica 0.5%, sodium carbonate 10%, rare earth 0.1%, anthraquinone analog compound
1%, remaining is water.
The nano-titanium dioxide is that partial size is 50nm, and nano silica partial size is 40nm, and sodium carbonate is lightweight carbon
Sour sodium, rare earth are ion adsorption type re, and anthraquinone compounds are dissociated anthraquinone, and the dissociated anthraquinone is Physcion.
A kind of preparation method of nanocomposite degumming and refining agent of the present invention, comprising the following steps:
(1) use the dedicated high shear dispersion machine of nano material, adjustment revolution be 5000 revs/min, by nano-titanium dioxide with
High speed shear is carried out after the one third mixing of water inventory and disperses 5min, discharges and A liquid is made；
(2) the dedicated high shear dispersion machine of nano material is used, adjustment revolution is 5000 revs/min, takes proper amount of nano titanium dioxide
Silicon carries out high speed shear dispersion 5min after mixing with the one third of water inventory, discharge and B liquid is made；
(3) A liquid and B liquid are uniformly mixed under agitation, obtain nanocomposite, discharged spare；
(4) after mixing rare earth with the one third of water inventory, anthraquinone analog compound is added under stirring conditions, rotates forward stirring
10min, then stirring 5min discharging is inverted, C liquid is made；
(5) nanocomposite and C liquid are subjected to homogeneous under agitation, D liquid is made after mixing evenly；
(6) sodium carbonate is added into D liquid under agitation, adjusting pH is 10-13, under stirring conditions by solution temperature liter
Up to 45 DEG C, after being stirred to react 20min, supernatant is removed by centrifugation, lower sediment particle is made into precipitating by ultrasound
Grain is uniformly dispersed, and the discharging of 0.2-0.3mm powder particle, as the nanocomposite degumming catalyst is made.
Embodiment 3
A kind of nanocomposite degumming and refining agent, the nanocomposite degumming catalyst is by following weight percent
Raw material is prepared: nano-titanium dioxide 3%, nano silica 2%, sodium carbonate 20%, rare earth 2%, anthraquinone analog compound 3%,
Yu Weishui.
The nano-titanium dioxide is that partial size is 60nm, and nano silica partial size is 50nm, and sodium carbonate is lightweight carbon
Sour sodium, rare earth are ion adsorption type re, and anthraquinone compounds are dissociated anthraquinone, and the dissociated anthraquinone is aloe-emodin.
A kind of preparation method of nanocomposite degumming and refining agent of the present invention, comprising the following steps:
(1) use the dedicated high shear dispersion machine of nano material, adjustment revolution be 6000 revs/min, by nano-titanium dioxide with
High speed shear is carried out after the one third mixing of water inventory and disperses 10min, discharges and A liquid is made；
(2) the dedicated high shear dispersion machine of nano material is used, adjustment revolution is 6000 revs/min, takes proper amount of nano titanium dioxide
Silicon carries out high speed shear dispersion 10min after mixing with the one third of water inventory, discharge and B liquid is made；
(3) A liquid and B liquid are uniformly mixed under agitation, obtain nanocomposite, discharged spare；
(4) after mixing rare earth with the one third of water inventory, anthraquinone analog compound is added under stirring conditions, rotates forward stirring
15min, then stirring 6min discharging is inverted, C liquid is made；
(5) nanocomposite and C liquid are subjected to homogeneous under agitation, D liquid is made after mixing evenly；
(6) sodium carbonate is added into D liquid under agitation, adjusting pH is 10-13, under stirring conditions by solution temperature liter
Up to 50 DEG C, after being stirred to react 30min, supernatant is removed by centrifugation, lower sediment particle is made into precipitating by ultrasound
Grain is uniformly dispersed, and the discharging of 0.2-0.3mm powder particle, as the nanocomposite degumming catalyst is made.
Embodiment 4
A kind of nanocomposite degumming and refining agent, the nanocomposite degumming catalyst is by following weight percent
Raw material is prepared: nano-titanium dioxide 10%, nano silica 5%, sodium carbonate 40%, rare earth 10%, anthraquinone analog compound
10%, remaining is water.
The nano-titanium dioxide is that partial size is 80nm, and nano silica partial size is 70nm, and sodium carbonate is lightweight carbon
Sour sodium, rare earth are ion adsorption type re, and anthraquinone compounds are dissociated anthraquinone, and the dissociated anthraquinone is Rhein.
A kind of preparation method of nanocomposite degumming and refining agent of the present invention, comprising the following steps:
(1) use the dedicated high shear dispersion machine of nano material, adjustment revolution be 10000 revs/min, by nano-titanium dioxide with
High speed shear is carried out after the one third mixing of water inventory and disperses 30min, discharges and A liquid is made；
(2) the dedicated high shear dispersion machine of nano material is used, adjustment revolution is 10000 revs/min, takes proper amount of nano titanium dioxide
Silicon carries out high speed shear dispersion 30min after mixing with the one third of water inventory, discharge and B liquid is made；
(3) A liquid and B liquid are uniformly mixed under agitation, obtain nanocomposite, discharged spare；
(4) after mixing rare earth with the one third of water inventory, anthraquinone analog compound is added under stirring conditions, rotates forward stirring
30min, then stirring 10min discharging is inverted, C liquid is made；
(5) nanocomposite and C liquid are subjected to homogeneous under agitation, D liquid is made after mixing evenly；
(6) sodium carbonate is added into D liquid under agitation, adjusting pH is 10-13, under stirring conditions by solution temperature liter
Up to 60 DEG C, after being stirred to react 50min, supernatant is removed by centrifugation, lower sediment particle is made into precipitating by ultrasound
Grain is uniformly dispersed, and the discharging of 0.2-0.3mm powder particle, as the nanocomposite degumming catalyst is made.
Comparative example 1
Comparative example 1 the difference from embodiment 1 is that, be not added with nano-titanium dioxide in comparative example 1.
Comparative example 2
Comparative example 2 the difference from embodiment 1 is that, be not added with anthraquinone analog compound in comparative example 2.
Comparative example 3
Comparative example 3 the difference from embodiment 1 is that, be not added with rare earth in comparative example 3.
Degumming catalyst made from embodiment 1-4 and comparative example 1-3 is applied in degumming tech, by degumming catalyst
To carry out being mixed to prepare mixed solution with the mass ratio of water 1:20, silk fabric is added in mixed solution and is carried out at degumming
Reason, wherein bath raio is 1:10, and silk fabric carries out following performance test by treated, and test result is as shown in table 1.
The measurement of mechanical strength: the silk fabric after degumming is dried to constant weight in baking oven (105 DEG C), moves to perseverance rapidly
After balancing for 24 hours between constant temperature and humidity, it is cut into 25 cm long.Test condition are as follows: 100 mm of sample holder length, 100 mm/ of tensile speed
Min, pretension (0.05 ± 0.01) cN/dtex, temperature (20 ± 2) DEG C, relative humidity (65 ± 5) %.
Degumming rate measures: the silk fabric for being 30% by relative humidity, and the weight before and after its degumming is measured at a temperature of 25 DEG C
Amount, according to the weight of poor quality divided by fabric before degumming weighed twice, as degumming rate.
It is obtained from table 1, nanocomposite, which is made, in the present invention has good degumming effect to silk fabric, changes simultaneously
Property mixing nanofiller crucial effect is played to the degumming of silk fabric, and carry out degumming using the nanocomposite
Afterwards, silk fabric still maintains good mechanical strength, does not generate destructive influences to the mechanical property of fabric, and add
Add the nanocomposite of anthraquinone analog compound and rare earth to silk fabric processing after with un-added compared with degumming effect more preferably,
Color more brilliant white, to illustrate that anthraquinone analog compound and rare earth compounding play the role of certain degumming and improve bleaching effect
Effect.Therefore nanocomposite degumming catalyst produced by the present invention is with a wide range of applications in degumming tech.
Table 1
| Test index | Comparative example before degumming | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Breaking strength (cN/dtex) | 4.86 | 4.84 | 4.79 | 4.80 | 4.82 | 4.79 | 4.81 | 4.81 |
| Elongation at break (%) | 78.2 | 75.6 | 74.2 | 74.8 | 75.3 | 75.4 | 75.3 | 75.4 |
| Degumming rate (%) | - | 96.2 | 94.1 | 94.9 | 95.8 | 73.2 | 86.4 | 85.7 |
Claims (6)
1. a kind of nanocomposite degumming and refining agent, which is characterized in that the nanocomposite degumming catalyst by with
The raw material of lower weight percent is prepared: nano-titanium dioxide 1-10%, nano silica 0.5-5%, sodium carbonate 10-40%,
Rare earth 0.1-10%, anthraquinone analog compound 1-10%, remaining is water.
2. a kind of nanocomposite degumming and refining agent according to claim 1, which is characterized in that described is nano combined
Material degumming catalyst is prepared by the raw material of following weight percent: nano-titanium dioxide 5%, nano silica 3%, carbon
Sour sodium 25%, rare earth 5%, anthraquinone analog compound 5%, remaining is water.
3. a kind of nanocomposite degumming and refining agent according to claim 1, which is characterized in that the nano-silica
Change titanium is that partial size is 50-80nm, and nano silica partial size is 40-70nm, and sodium carbonate is light sodium carbonate, and rare earth is ion suction
Attached type rare earth, anthraquinone compounds are dissociated anthraquinone.
4. a kind of nanocomposite degumming and refining agent according to claim 1, which is characterized in that the dissociated anthraquinone
For one or more combinations of Chrysophanol, rheum emodin, Physcion, aloe-emodin or Rhein.
5. a kind of described in any item preparation methods of nanocomposite degumming and refining agent of claim 1-4, which is characterized in that
The following steps are included:
(1) the dedicated high shear dispersion machine of nano material is used, adjustment revolution is 5000-10000 revs/min, by nano-silica
Change and carry out high speed shear dispersion 5-30min after titanium is mixed with the one third of water inventory, discharges and A liquid is made；
(2) the dedicated high shear dispersion machine of nano material is used, adjustment revolution is 5000-10000 revs/min, takes proper amount of nano
Silica carries out high speed shear dispersion 5-30min after mixing with the one third of water inventory, discharge and B liquid is made；
(3) A liquid and B liquid are uniformly mixed under agitation, obtain nanocomposite, discharged spare；
(4) after mixing rare earth with the one third of water inventory, anthraquinone analog compound is added under stirring conditions, rotates forward stirring
10-30min, then stirring 5-10min discharging is inverted, C liquid is made；
(5) nanocomposite and C liquid are subjected to homogeneous under agitation, D liquid is made after mixing evenly；
(6) sodium carbonate is added into D liquid under agitation, adjusting pH is 10-13, under stirring conditions by solution temperature liter
Up to 45-60 DEG C, after being stirred to react 20-50min, supernatant is removed by centrifugation, lower sediment particle is made by ultrasound
Precipitating particle is uniformly dispersed, and the discharging of 0.2-0.3mm powder particle, as the nanocomposite degumming catalyst is made.
6. a kind of application of the described in any item nanocomposite degumming and refining agent of claim 1-4 in degumming tech.
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Application publication date: 20190215 |