CN109371597A - A kind of preparation method of acid leach processing method and high silica glass fiber yarns rope - Google Patents
A kind of preparation method of acid leach processing method and high silica glass fiber yarns rope Download PDFInfo
- Publication number
- CN109371597A CN109371597A CN201811344051.0A CN201811344051A CN109371597A CN 109371597 A CN109371597 A CN 109371597A CN 201811344051 A CN201811344051 A CN 201811344051A CN 109371597 A CN109371597 A CN 109371597A
- Authority
- CN
- China
- Prior art keywords
- rope
- silvalin
- acid
- creel
- acid leach
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
- D06B3/04—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of yarns, threads or filaments
- D06B3/09—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of yarns, threads or filaments as packages, e.g. cheeses
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B1/00—Applying liquids, gases or vapours onto textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing or impregnating
- D06B1/02—Applying liquids, gases or vapours onto textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing or impregnating by spraying or projecting
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B15/00—Removing liquids, gases or vapours from textile materials in association with treatment of the materials by liquids, gases or vapours
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B23/00—Component parts, details, or accessories of apparatus or machines, specially adapted for the treating of textile materials, not restricted to a particular kind of apparatus, provided for in groups D06B1/00 - D06B21/00
- D06B23/04—Carriers or supports for textile materials to be treated
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Surface Treatment Of Glass Fibres Or Filaments (AREA)
- Ropes Or Cables (AREA)
Abstract
The present invention relates to field of inorganic materials, more particularly to a kind of acid leach processing method and the preparation method of high silica glass fiber yarns rope, wherein, the acid leach processing method of the silvalin rope is that the silvalin rope is wound on creel, then the creel for winding silvalin rope is placed in acid solution, and it is rotated in acid solution, to realize that acid leach reacts, the acid solution is hydrochloric acid, one of nitric acid or sulfuric acid are several, acid leaching process of the invention is rotated in acid solution by creel, make to generate forced convertion between yarn and acid solution, be conducive to improve silica content uniformity, reduce the coefficient of variation and the strength coefficient of variation of the silica content of the high silica glass fiber yarns rope between batch, improve the quality and production efficiency of product.
Description
Technical field
The present invention relates to field of inorganic materials, and in particular to a kind of acid leach processing method and high silica glass fiber yarns rope
Preparation method.
Background technique
With the progress and development of aerospace science technology, requirement of the people to high temperature resistant wave-permeable heat-barrier material be not yet
Disconnected to improve, traditional high temperature resistant heat insulation material such as asbestos, rock wool etc. is no longer satisfied high standard since thermal coefficient is higher
It is required that.Resurrection glass fibre is a kind of high-temperature-resistant inorganic fibre, with softening point is high, thermal coefficient is low, wave is good etc.
The characteristics of and be increasingly subject to extensive concern.
In the prior art, resurrection glass fibre is mostly with alkali-free glass fibre, binary glass fiber or TERNARY GLASS
Fiber is that raw material is made by acid leach, washing, drying and sintering, in this technical process, although producer increasingly reinforces to acid
The control of the parameters such as number, the time washed in acid concentration, treatment temperature and processing time and water-washing process in Leaching process
System, however final high silica fiber obtained still has the problem of irregular, product the stability difference of quality, especially by force
Degree, silica content fluctuation are larger, are unable to satisfy requirement.
In the prior art, resurrection glass fibre generallys use the mode for standing suspension during acid leach, for example, in
State patent document CN101654833A discloses a kind of high silica glass fiber staple-yarn and its manufacturing process, using hang
Yarn is placed in acid leach slot, acid solution is heated directly into acid leach slot using steam, then carries out spray cleaning spent acid, later
Directly carry out thermal finalization processing；Chinese patent literature CN102839476A discloses a kind of life of high-strength high silica glass fiber yarns
Yarn is placed in acid leach slot by production. art using hang, the hydrochloric acid short time acid leach of first 0.3~0.5N of low concentration,
The hydrochloric acid long-time acid leach of 2.0~3.2N of high concentration again, point 2 steps complete acid leach, using steam directly into acid leach slot
Acid solution is heated, then carries out spray cleaning spent acid, directly carries out thermal finalization processing later.
However, due in the above technology yarn be placed in acid leach slot with hang, by acid-proof pump to acid solution into
Row stirring, causes acid solution and each location contacts of yarn uneven, and is unable to the chemical reaction of stability contorting acid leach, so that being made
High silica fiber yarn rope in silica content it is uneven；Meanwhile also resulting in yarn and being unable to fully spray and wash, it reduces
Production efficiency influences the consistency of product quality, especially makes the strength coefficient of variation of product between different batches excessive, Wu Fashi
Answer the application requirement of the high-end fields such as aerospace.
Summary of the invention
Therefore, the technical problem to be solved in the present invention is that overcoming the high silica glass fiber yarns rope prepared in the prior art
The defect that quality conformance is poor, production efficiency is low, to provide a kind of acid leach processing method and high silica glass fiber yarns rope
Preparation method.
The present invention provides a kind of acid leach processing methods of silvalin rope, and the silvalin rope is wound on creel,
Then the creel for winding silvalin rope is placed in acid solution, and is rotated in acid solution, to realize that acid leach reacts.
The acid solution is hydrochloric acid, one of nitric acid or sulfuric acid or several.
The section of the creel is regular polygon structure made of body of rod support, and the silvalin rope is to wind than for 2-
10, specification of the thickness no more than 3cm is wound on the body of rod.
The number of edges of the regular polygon structure in the section of the creel is 3-30.
The radius of the circumscribed circle of the creel is 15cm-1000cm.
The rotation refers to that the creel for being wound with silvalin rope is rotated around the central axis of creel, and velocity of rotation is
5-80rpm。
Indirect heating is carried out to the acid solution.
The equivalent concentration of the acid solution is 1.0-3.6N/L, and temperature is 80-100 DEG C, and the creel for being wound with silvalin rope exists
The time rotated in acid solution is 60-150min.
The silvalin rope can be, but not limited to alkali-free glass fibre yarn rope, Shift of Binary Sodium Silicate glass fiber yarn rope or three
One of first sodium borosilicate glass fiber yarn rope or in which it is several, the silvalin rope may be other glass fibres
Yarn rope.
When silvalin rope is alkali-free glass fibre yarn rope, acid strength 1.0-2.5N/L, 80-90 DEG C of temperature, acidleach
Drip time 60-90min.When silvalin rope is Shift of Binary Sodium Silicate glass fiber yarn rope or tribasic sodium borosilicate fiberglass yarn
When rope, acid strength 2.4-3.6N/L, 90-100 DEG C of temperature, acidleach drip time 90-150min.
The present invention also provides a kind of preparation method of high silica glass fiber yarns rope, the acid including the silvalin rope
Leaching processing method.
It further include acid leach preprocessing process before acid leach processing, in the acid leach preprocessing process, acid
The equivalent concentration of liquid is 1.4-3.6N/L, and temperature is 50-80 DEG C, and the processing time is 10-60min.
It further include that spray washing and soaking and water washing are carried out to acid leach treated silvalin rope, until the silvalin rope
The pH value on surface is 6 or more.
After the completion of acid leach processing, maintain to carry out spray process to silvalin rope surface with water while creel rotation, with
Realize the process of spray washing.
Creel rotation is maintained, the creel for being wound with silvalin rope is dipped in the process for realizing soaking and water washing in water.
During the spray washing and soaking and water washing, the temperature of water is 60-80 DEG C, and the revolving speed of creel is 15-30rpm,
Wherein, the number of spray washing is 2-4 times, each 5-10min, and the number of soaking and water washing is 2-3 times, each 25-35min, and
The spray washing and soaking and water washing are alternately.
Further include the steps that the water of silvalin rope adsorption after going down at 100-150 DEG C except washing process.
Further include that single yarn rope is soaked in post-treatment agent, carries out surface dipping process, be subsequently placed at 150-350 DEG C and dry
The step of dry film forming.
Technical solution of the present invention has the advantages that
1. the preparation method of high silica glass fiber yarns rope provided by the invention, by using creel drive silvalin rope with
Rotating manner, which contact with the acid solution in acid leach slot, occurs acid leach reaction, makes to generate pressure pair between yarn and acid solution
Stream, be conducive to improve silica content uniformity, improve the quality of product, compared with the prior art in yarn with stand suspension
Mode is placed in acid leach slot, can be substantially reduced the change of the silica content in the high silica glass fiber yarns rope between batch
Different coefficient and the strength coefficient of variation, the uniformity of product are improved, and by the way that silvalin rope to be wound on creel, are supported
The shape of the body of rod is any can be loosened in right amount as needed according to the winding tension size of yarn on one side, reduce yarn winding tension, reduced
Acidleach drips chemical reaction process to the mechanical damage of yarn, to improve yarn mechanics stability；Further pass through creel
While driving yarn rotation, realizes spray washing and soaking and water washing, be further ensured that the efficiency and quality of washing, it can be into one
Step reduces the coefficient of variation and the strength coefficient of variation of the silica content in the high silica glass fiber yarns rope between batch, improves life
Produce efficiency.
2. the preparation method of high silica glass fiber yarns rope provided by the invention, by fine in control acid leach treatment process
The winding of dimension yarn rope compares for 2-10, can not only improve because winding than too greatly due to cause the angle of the crossing between yarn too small, and make
The problem of flow effect is deteriorated between yarn layer, acid leach reaction effect is deteriorated at acid solution can also improve due to winding than too small
Cause the angle of the crossing between yarn excessive, and yarn is made to occur at random after acid leach and be unfavorable for further spraying water washing, thus
Further increase the homogeneity of product quality；On the other hand, since the cross-sectional shape of creel determines silvalin rope and creel
Contact points, by using section be the creel with the regular polygon structure of number of edges between 3-30 can not only improve
Creel with silvalin rope contact point is too small that it is made easily to occur at random after with rotating manner acid leach and influence water washing effect
It happens, can also reduce the acid leach time, improve the quality of acid leach reaction, it is little by the thickness for controlling silvalin rope
In 3cm, the consistency of quality can be further increased, guarantees the stability of acid leach processing, realizes high silica glass fiber yarns
The uniformity of silica content in rope.
3. the preparation method of high silica glass fiber yarns rope provided by the invention, by using heat exchanger to acid leach slot
Interior acid solution carries out indirect heating, avoids constantly being passed through Steam dilution acid solution into acid leach slot in the prior art and makes acid leach
The case where concentration of middle acid solution constantly reduces and is unfavorable for the control to production technology and product quality appearance, also improves simultaneously
The phenomenon that unevenly being heated up by steam direct heating bring acid solution, and then the effect of acid leach reaction is improved, further
Improve the uniformity of silica content in high silica glass fiber yarns rope.
4. the preparation method of high silica glass fiber yarns rope provided by the invention, by single fiber yarn rope successively impregnation,
Instead of whole group's cotton yarn while impregnation, being conducive to every silvalin rope 360 ° omni-directional, impregnation rod squeezes guarantee glue infiltration yarn simultaneously
Line internal layer and coating uniformity, are placed in drying and forming-film at 150-350 DEG C, improve coating quality.
5. the preparation method of high silica glass fiber yarns rope provided by the invention, the washing process process is to pass through spray
Washing and soaking and water washing alternately, can further increase the quality of water-washing process, improve the homogeneity of product.
Specific embodiment
There is provided following embodiments is to preferably further understand the present invention, it is not limited to the best embodiment party
Formula is not construed as limiting the contents of the present invention and protection scope, anyone under the inspiration of the present invention or by the present invention and its
The feature of his prior art is combined and any and identical or similar product of the present invention for obtaining, all falls within of the invention
Within protection scope.
Following embodiment, dibasic sodium borosilicate fiberglass yarn rope used, tribasic sodium borosilicate fiberglass yarn rope
It is Zhongcai Sci. & Tech. Co., Ltd's production, alkali-free glass fibre yarn rope is Shandong Fiberglass Group Co., Ltd.'s production,
Specific experiment step or condition person are not specified in embodiment, according to the literature in the art the behaviour of described routine experiment step
Work or condition can carry out.Reagents or instruments used without specified manufacturer is that can be tried by the routine of commercially available acquisition
Agent product.
Embodiment 1
The preparation method for present embodiments providing a kind of high silica glass fiber yarns rope, includes the following steps: acid leach, water
It washes, dry, be sintered and be surface-treated, concrete operations are as follows:
Acid leach: by tribasic sodium borosilicate fiberglass yarn rope (specification: BC8-220S120) with wind than for 3.14 around
On acidproof creel, wherein the creel section of selection is positive hexagonal structure, and the radius of the circumscribed circle of creel is 500cm, winding
Silvalin rope yarn layer with a thickness of 2.6cm, then creel is rotationally connected in acid leach slot by shaft；It is dense using equivalent
The hydrochloric acid solution is injected in resistance to heat exchanger after being heated to 50 DEG C as acid solution and injects acid by the hydrochloric acid solution that degree is 3.1N/L
In leaching tank；Then starting creel rotation, control creel velocity of rotation is 20rpm, while the acid solution in acid leach slot being passed through again
It crosses in pump input heat exchanger and carries out circulating-heating, until the temperature of acid solution is 95 DEG C, then maintaining acid liquor temperature is at 95 DEG C
Insulation reaction 100min.
Washing: after acid leach, the acid solution in acid leach slot being discharged, and the silvalin rope after acid leach is dried,
Be subsequently placed in acid leach slot, control creel and rotated with the speed of 20rpm, at the same with 62 DEG C of water to the surface of silvalin rope into
Then row spray washing 10min injects 62 DEG C of water to silvalin rope soaking and water washing 30min into acid leach slot, draining finishes, leaching
The water adsorbed in dry fibers yarn rope, control creel is rotated again with the speed of 20rpm later, while with 62 DEG C of water to silvalin
The surface of rope carries out spray washing 10min, and 62 DEG C of water is then injected into acid leach slot to silvalin rope soaking and water washing
30min, the pH value for measuring silvalin rope surface at this time is 6.8, and washing is completed.
Drying and sintering: the silvalin rope after washing being placed at 120 DEG C and dries 90min, removes the moisture of adsorption,
Then first sintering is carried out, rises to 600 DEG C from 120 DEG C with the heating rate of 6 DEG C/min, then keeps the temperature 30min, then carry out two
Secondary sintering is continued to be warming up to 730 DEG C from 600 DEG C with the heating rate of 4 DEG C/min, then keeps the temperature 30min, then naturally cool to
Room temperature, sintering finish.
Surface treatment: it using in the glue that single fiber yarn rope passes through steeping vat respectively and is immersed in steeping vat, carries out
Abundant impregnation, the glue are reinforced resins glue, are then dried in 150 DEG C of drying oven, then are rolled up with dividing sinker winding apparatus
Around molding, high silica glass fiber yarns rope is made.
Acid leach, washing, drying and sintering, the surface treatment for repeating 5 rounds using the technique, are prepared 5
The high silica glass fiber yarns rope of different batches.
Embodiment 2
The preparation method for present embodiments providing a kind of high silica glass fiber yarns rope, includes the following steps: acid leach, water
It washes, dry, be sintered and be surface-treated, concrete operations are as follows:
Acid leach: by tribasic sodium borosilicate fiberglass yarn rope (specification: BC8-440S120) with wind than for 9.84 around
On acidproof creel, wherein the creel section of selection is positive pentagonal configuration, and the radius of the circumscribed circle of creel is 15cm, winding
Silvalin rope yarn layer with a thickness of 1.8cm, then creel is rotationally connected in acid leach slot by shaft；It is dense using equivalent
The hydrochloric acid solution is injected in resistance to heat exchanger after being heated to 50 DEG C as acid solution and injects acid by the hydrochloric acid solution that degree is 3.5N/L
In leaching tank；Then starting creel rotation, control creel velocity of rotation is 50rpm, while the acid solution in acid leach slot being passed through again
It crosses in pump input heat exchanger and carries out circulating-heating, until the temperature of acid solution is 90 DEG C, then maintaining acid liquor temperature is at 90 DEG C
Insulation reaction 150min.
Washing: after acid leach, the acid solution in acid leach slot being discharged, and the silvalin rope after acid leach is dried,
Be subsequently placed in acid leach slot, control creel and rotated with the speed of 15rpm, at the same with 80 DEG C of water to the surface of silvalin rope into
Then row spray washing 5min injects 80 DEG C of water to silvalin rope soaking and water washing 25min into acid leach slot, draining finishes, leaching
The water adsorbed in dry fibers yarn rope, carries out spray washing next time and soaking and water washing process again later, until measurement silvalin rope
The pH on surface is 6.8, and washing finishes, and is carried out spray washing 4 times, soaking and water washing 3 times altogether.
Drying and sintering: the silvalin rope after washing is placed at 110 DEG C and dries 100min, removes the water of adsorption
Point, first sintering is then carried out, rises to 600 DEG C from 120 DEG C with the heating rate of 6 DEG C/min, then keeps the temperature 30min, then into
Row double sintering is continued to be warming up to 730 DEG C from 600 DEG C with the heating rate of 4 DEG C/min, then keeps the temperature 30min, then naturally cold
But to room temperature, sintering is finished.
Surface treatment: it using in the glue that single fiber yarn rope passes through steeping vat respectively and is immersed in steeping vat, carries out
Abundant impregnation, the glue are reinforced resins glue, are then dried in 220 DEG C of drying oven, then are rolled up with dividing sinker winding apparatus
Around molding, high silica glass fiber yarns rope is made.
Acid leach, washing, drying and sintering, the surface treatment for repeating 5 rounds using the technique, are prepared 5
The high silica glass fiber yarns rope of different batches.
Embodiment 3
The preparation method for present embodiments providing a kind of high silica glass fiber yarns rope, includes the following steps: acid leach, water
It washes, dry, be sintered and be surface-treated, concrete operations are as follows:
Acid leach: by tribasic sodium borosilicate fiberglass yarn rope (specification: BC8-440S120) with wind than for 2.16 around
On acidproof creel, wherein the creel section of selection is positive three decagons, and the radius of the circumscribed circle of creel is 1000cm, winding
Silvalin rope yarn layer with a thickness of 3cm, then creel is rotationally connected in acid leach slot by shaft；Use equivalent concentration
For 2.4N/L hydrochloric acid solution as acid solution, which is injected in resistance to heat exchanger after being heated to 80 DEG C and injects acid drip
In filter pocket；Then the rotation of starting creel, control creel velocity of rotation are 5rpm, while by the acid solution in acid leach slot using pump
Circulating-heating is carried out in input heat exchanger, until the temperature of acid solution is 100 DEG C, then maintaining acid liquor temperature is to protect at 100 DEG C
Temperature reaction 90min.
Washing: after acid leach, the acid solution in acid leach slot being discharged, and the silvalin rope after acid leach is dried,
Be subsequently placed in acid leach slot, control creel and rotated with the speed of 25rpm, at the same with 60 DEG C of water to the surface of silvalin rope into
Then row spray washing 10min injects 60 DEG C of water to silvalin rope soaking and water washing 35min into acid leach slot, draining finishes, leaching
The water adsorbed in dry fibers yarn rope, carries out spray washing next time and soaking and water washing process again later, until measurement silvalin rope
The pH on surface is 6.4, and washing finishes, and is carried out spray washing 3 times, soaking and water washing 3 times altogether.
Drying and sintering: the silvalin rope after washing being placed at 150 DEG C and dries 80min, removes the moisture of adsorption,
Then first sintering is carried out, rises to 600 DEG C from 120 DEG C with the heating rate of 6 DEG C/min, then keeps the temperature 30min, then carry out two
Secondary sintering is continued to be warming up to 730 DEG C from 600 DEG C with the heating rate of 4 DEG C/min, then keeps the temperature 30min, then naturally cool to
Room temperature, sintering finish.
Surface treatment: it using in the glue that single fiber yarn rope passes through steeping vat respectively and is immersed in steeping vat, carries out
Abundant impregnation, the glue are reinforced resins glue, are then dried in 150 DEG C of drying oven, then are rolled up with dividing sinker winding apparatus
Around molding, high silica glass fiber yarns rope is made.
Acid leach, washing, drying and sintering, the surface treatment for repeating 5 rounds using the technique, are prepared 5
The high silica glass fiber yarns rope of different batches.
Embodiment 4
The preparation method for present embodiments providing a kind of high silica glass fiber yarns rope, includes the following steps: acid leach, water
It washes, dry, be sintered and be surface-treated, concrete operations are as follows:
Acid leach: by tribasic sodium borosilicate fiberglass yarn rope (specification: BC8-220S120) to wind than for 12.41
It is wound on acidproof creel, wherein the creel section of selection is positive triangular structure, and the radius of the circumscribed circle of creel is 500cm, volume
Around silvalin rope yarn layer with a thickness of 2.6cm, then creel is rotationally connected in acid leach slot by shaft；Use equivalent
The hydrochloric acid solution is injected in resistance to heat exchanger after being heated to 50 DEG C and is injected as acid solution by the hydrochloric acid solution that concentration is 3.1N/L
In acid leach slot；Then starting creel rotation, control creel velocity of rotation are 20rpm, while again by the acid solution in acid leach slot
By carrying out circulating-heating in pump input heat exchanger, until the temperature of acid solution is 95 DEG C, then maintaining acid liquor temperature is 95 DEG C
Lower insulation reaction 100min.
Washing: after acid leach, the acid solution in acid leach slot being discharged, and the silvalin rope after acid leach is dried,
Be subsequently placed in acid leach slot, control creel and rotated with the speed of 20rpm, at the same with 62 DEG C of water to the surface of silvalin rope into
Then row spray washing 10min injects 62 DEG C of water to silvalin rope soaking and water washing 30min into acid leach slot, draining finishes, and squeezes
The water adsorbed in dry fibers yarn rope, control creel is rotated again with the speed of 20rpm later, while with 62 DEG C of water to silvalin
The surface of rope carries out spray washing 10min, and 62 DEG C of water is then injected into acid leach slot to silvalin rope soaking and water washing
30min, the pH value for measuring silvalin rope surface at this time is 6.8, and washing is completed.
Drying and sintering: the silvalin rope after washing being placed at 120 DEG C and dries 90min, removes the moisture of adsorption,
Then first sintering is carried out, rises to 600 DEG C from 120 DEG C with the heating rate of 6 DEG C/min, then keeps the temperature 30min, then carry out two
Secondary sintering is continued to be warming up to 730 DEG C from 600 DEG C with the heating rate of 4 DEG C/min, then keeps the temperature 30min, then naturally cool to
Room temperature, sintering finish.
Surface treatment: it using in the glue that single fiber yarn rope passes through steeping vat respectively and is immersed in steeping vat, carries out
Abundant impregnation, the glue are reinforced resins glue, are then dried in 150 DEG C of drying oven, then are rolled up with dividing sinker winding apparatus
Around molding, high silica glass fiber yarns rope is made.
Acid leach, washing, drying and sintering, the surface treatment for repeating 5 rounds using the technique, are prepared 5
The high silica glass fiber yarns rope of different batches.
Embodiment 5
The preparation method for present embodiments providing a kind of high silica glass fiber yarns rope, includes the following steps: acid leach, water
It washes, dry, be sintered and be surface-treated, concrete operations are as follows:
Acid leach: by tribasic sodium borosilicate fiberglass yarn rope (specification: BC8-220S120) with wind than for 3.14 around
On acidproof creel, wherein the creel section of selection is positive hexagonal structure, and the radius of the circumscribed circle of creel is 500cm, winding
Silvalin rope yarn layer with a thickness of 2.6cm, then creel is rotationally connected in acid leach slot by shaft；It is dense using equivalent
The hydrochloric acid solution that degree is 3.1N/L injects the hydrochloric acid solution in acid leach slot as acid solution；Then starting creel rotation, control
Creel velocity of rotation is 20rpm, while being passed through steam into acid leach slot and directly heating to acid solution, until the temperature of acid solution
It is 95 DEG C, then maintaining acid liquor temperature is insulation reaction 100min at 95 DEG C.
Washing: after acid leach, the acid solution in acid leach slot being discharged, and the silvalin rope after acid leach is dried,
Be subsequently placed in acid leach slot, control creel and rotated with the speed of 20rpm, at the same with 62 DEG C of water to the surface of silvalin rope into
Then row spray washing 10min injects 62 DEG C of water to silvalin rope soaking and water washing 30min into acid leach slot, draining finishes, and squeezes
The water adsorbed in dry fibers yarn rope, control creel is rotated again with the speed of 20rpm later, while with 62 DEG C of water to silvalin
The surface of rope carries out spray washing 10min, and 62 DEG C of water is then injected into acid leach slot to silvalin rope soaking and water washing
30min, the pH value for measuring silvalin rope surface at this time is 6.8, and washing is completed.
Drying and sintering: the silvalin rope after washing being placed at 120 DEG C and dries 90min, removes the moisture of adsorption,
Then first sintering is carried out, rises to 600 DEG C from 120 DEG C with the heating rate of 6 DEG C/min, then keeps the temperature 30min, then carry out two
Secondary sintering is continued to be warming up to 730 DEG C from 600 DEG C with the heating rate of 4 DEG C/min, then keeps the temperature 30min, then naturally cool to
Room temperature, sintering finish.
Surface treatment: it using in the glue that single fiber yarn rope passes through steeping vat respectively and is immersed in steeping vat, carries out
Abundant impregnation, the glue are reinforced resins glue, are then dried in 150 DEG C of drying oven, then are rolled up with dividing sinker winding apparatus
Around molding, high silica glass fiber yarns rope is made.
Acid leach, washing, drying and sintering, the surface treatment for repeating 5 rounds using the technique, are prepared 5
The high silica glass fiber yarns rope of different batches.
Embodiment 6
The preparation method for present embodiments providing a kind of high silica glass fiber yarns rope, includes the following steps: acid leach, water
It washes, dry, be sintered and be surface-treated, concrete operations are as follows:
Acid leach: by alkali-free glass fibre yarn rope (specification: EC8-220S120) to wind than being wound on acidproof creel for 3.14
On, wherein the creel section of selection is positive hexagonal structure, and the radius of the circumscribed circle of creel is 500cm, the silvalin rope of winding
Yarn layer with a thickness of 2.6cm, then creel is rotationally connected in acid leach slot by shaft；It the use of equivalent concentration is 3.1N/L
Hydrochloric acid solution as acid solution, which is injected in resistance to heat exchanger after being heated to 50 DEG C and is injected in acid leach slot；
Then starting creel rotation, control creel velocity of rotation are 20rpm, while by the acid solution in acid leach slot using pump input heat
Circulating-heating is carried out in exchanger, until the temperature of acid solution is 90 DEG C, then maintaining acid liquor temperature is insulation reaction at 90 DEG C
100min。
Washing: after acid leach, the acid solution in acid leach slot being discharged, and the silvalin rope after acid leach is dried,
Be subsequently placed in acid leach slot, control creel and rotated with the speed of 20rpm, at the same with 62 DEG C of water to the surface of silvalin rope into
Then row spray washing 10min injects 62 DEG C of water to silvalin rope soaking and water washing 30min into acid leach slot, draining finishes, leaching
The water adsorbed in dry fibers yarn rope, control creel is rotated again with the speed of 20rpm later, while with 62 DEG C of water to silvalin
The surface of rope carries out spray washing 10min, and 62 DEG C of water is then injected into acid leach slot to silvalin rope soaking and water washing
30min, the pH value for measuring silvalin rope surface at this time is 6.8, and washing is completed.
Drying and sintering: the silvalin rope after washing being placed at 120 DEG C and dries 90min, removes the moisture of adsorption,
Then first sintering is carried out, rises to 600 DEG C from 120 DEG C with the heating rate of 6 DEG C/min, then keeps the temperature 30min, then carry out two
Secondary sintering is continued to be warming up to 730 DEG C from 600 DEG C with the heating rate of 4 DEG C/min, then keeps the temperature 30min, then naturally cool to
Room temperature, sintering finish.
Surface treatment: it using in the glue that single fiber yarn rope passes through steeping vat respectively and is immersed in steeping vat, carries out
Abundant impregnation, the glue are reinforced resins glue, are then dried in 150 DEG C of drying oven, then are rolled up with dividing sinker winding apparatus
Around molding, high silica glass fiber yarns rope is made.
Acid leach, washing, drying and sintering, the surface treatment for repeating 5 rounds using the technique, are prepared 5
The high silica glass fiber yarns rope of different batches.
Embodiment 7
The preparation method for present embodiments providing a kind of high silica glass fiber yarns rope, includes the following steps: acid leach, water
It washes, dry, be sintered and be surface-treated, concrete operations are as follows:
Acid leach: by Shift of Binary Sodium Silicate glass fiber yarn rope (specification: AC8-220S120) to wind than being wound on for 3.14
On acidproof creel, wherein the creel section of selection is positive hexagonal structure, and the radius of the circumscribed circle of creel is 500cm, winding
Then creel is rotationally connected in acid leach slot by the yarn layer of silvalin rope with a thickness of 2.6cm by shaft；Use equivalent concentration
For 3.2N/L hydrochloric acid solution as acid solution, which is injected in resistance to heat exchanger after being heated to 50 DEG C and injects acid drip
In filter pocket；Then starting creel rotation, control creel velocity of rotation be 20rpm, while by the acid solution in acid leach slot using
Circulating-heating is carried out in pump input heat exchanger, until the temperature of acid solution is 85 DEG C, then maintaining acid liquor temperature is to protect at 85 DEG C
Temperature reacts 90min.
Washing: after acid leach, the acid solution in acid leach slot being discharged, and the silvalin rope after acid leach is dried,
Be subsequently placed in acid leach slot, control creel and rotated with the speed of 20rpm, at the same with 62 DEG C of water to the surface of silvalin rope into
Then row spray washing 10min injects 62 DEG C of water to silvalin rope soaking and water washing 30min into acid leach slot, draining finishes, leaching
The water adsorbed in dry fibers yarn rope, control creel is rotated again with the speed of 20rpm later, while with 62 DEG C of water to silvalin
The surface of rope carries out spray washing 10min, and 62 DEG C of water is then injected into acid leach slot to silvalin rope soaking and water washing
30min, the pH value for measuring silvalin rope surface at this time is 6.1, and washing is completed.
Drying and sintering: the silvalin rope after washing being placed at 120 DEG C and dries 90min, removes the moisture of adsorption,
Then first sintering is carried out, rises to 600 DEG C from 120 DEG C with the heating rate of 6 DEG C/min, then keeps the temperature 30min, then carry out two
Secondary sintering is continued to be warming up to 740 DEG C from 600 DEG C with the heating rate of 4 DEG C/min, then keeps the temperature 30min, then naturally cool to
Room temperature, sintering finish.
Surface treatment: it using in the glue that single fiber yarn rope passes through steeping vat respectively and is immersed in steeping vat, carries out
Abundant impregnation, the glue are reinforced resins glue, are then dried in 150 DEG C of drying oven, then are rolled up with dividing sinker winding apparatus
Around molding, high silica glass fiber yarns rope is made.
Acid leach, washing, drying and sintering, the surface treatment for repeating 5 rounds using the technique, are prepared 5
The high silica glass fiber yarns rope of different batches.
Comparative example 1
This comparative example provides a kind of preparation method of high silica glass fiber yarns rope, and preparation process is different with embodiment 1
Place is acid leach process.Acid leach process in this comparative example specifically: by tribasic sodium borosilicate fiberglass yarn rope (rule
Lattice: BC8-220S120) to wind than being wound on acidproof creel for 3.14, wherein the creel section of selection is regular hexagon knot
The radius of structure, the circumscribed circle of creel is 500cm, then creel is fixed on by the yarn layer of the silvalin rope of winding with a thickness of 2.6cm
In acid leach slot；Use the hydrochloric acid solution that equivalent concentration is 3.1N/L as acid solution, which is injected into acidproof heat exchange
It is injected in acid leach slot after being heated to 50 DEG C in device；Then it maintains creel motionless, two-way stirring is carried out to acid solution, mixing speed is
50rpm, while by the acid solution in acid leach slot using circulating-heating is carried out in pump input heat exchanger, until the temperature of acid solution
It is 95 DEG C, then maintaining acid liquor temperature is insulation reaction 100min at 95 DEG C.
Comparative example 2
This comparative example provides a kind of preparation method of high silica glass fiber yarns rope, and preparation process is different with embodiment 1
Place is acid leach process and water-washing process.Acid leach process in this comparative example specifically: by tribasic sodium borosilicate glass
Silvalin rope (specification: BC8-220S120) is to wind than being wound on acidproof creel for 3.14, wherein the creel section of selection is
Regular hexagon structure, the radius of the circumscribed circle of creel are 500cm, then the yarn layer of the silvalin rope of winding will with a thickness of 2.6cm
Creel is fixed in acid leach slot；Use the hydrochloric acid solution that equivalent concentration is 3.1N/L as acid solution, which is injected
It is injected in acid leach slot after being heated to 50 DEG C in resistance to heat exchanger；Then it maintains creel motionless, two-way stirring is carried out to acid solution,
Mixing speed is 50rpm, while the acid solution in acid leach slot being inputted in heat exchanger using pump and carries out circulating-heating, until
The temperature of acid solution is 95 DEG C, and then maintaining acid liquor temperature is insulation reaction 100min at 95 DEG C.
Water-washing process in this comparative example specifically: after by acid leach, the acid solution in acid leach slot is discharged, and will be sour
Silvalin rope drying after leaching, is subsequently placed in acid leach slot, control creel is motionless, while with 62 DEG C of water to silvalin rope
Surface carry out spray washing 10min, 62 DEG C of water are then injected into acid leach slot to silvalin rope soaking and water washing 30min, row
Water finishes, and the water adsorbed in leaching dry fibers yarn rope, secondary control is motionless again later, while with 62 DEG C of water to the surface of silvalin rope
Spray washing 10min is carried out, the water that 62 DEG C are then injected into acid leach slot surveys silvalin rope soaking and water washing 30min at this time
The pH value for determining silvalin rope surface is 5.3, and washing is completed.
Experimental example 1
Silica content survey is carried out to the high silica glass fiber yarns rope prepared in embodiment 1-7 and comparative example 1-2 respectively
Fixed, the results are shown in Table 1.
Silica content result in 1 high silica glass fiber yarns rope of table
Experimental example 2
Strength measurement is carried out to the high silica glass fiber yarns rope prepared in embodiment 1-7 and comparative example 1-2 respectively, respectively
The strength of the sample of five batches is measured, wherein random screening goes out 5 samples and measured respectively from each batch, is calculated
The strength coefficient of variation and batch interior strength coefficient of variation, the results are shown in Table shown in 2 between criticizing.
Table 2 embodiment 1-7 and comparative example 1-2 preparation high silica glass fiber yarns rope batch in strength and batch between strongly survey
Determine result
As can be seen from Table 1 and Table 2, compared with comparative example 1-2, the variation lines of the silica content in embodiment 1-7
Number, strength variation within batch coefficient and interassay coefficient of variation have significant decrease, wherein the coefficient of variation of silica content of the present invention
No more than 1.5%, strength variation within batch coefficient is not more than 13.2%, and interassay coefficient of variation is not more than 11.5%, compared with 1 He of comparative example
Comparative example 2 is substantially reduced, and illustrates that high silica glass fiber yarns rope quality of the invention is more reliable and more stable, homogeneity is obvious
It improves；Moreover, compared with embodiment 4 and 5, the silica content of high silica glass fiber yarns rope obtained in embodiment 1-3
The coefficient of variation, strength variation within batch coefficient and interassay coefficient of variation have significant decrease, and surface passes through to winding ratio, creel shape
And the optimization of heating method, be conducive to the stability for further increasing high silica glass fiber yarns rope quality obtained.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (16)
1. a kind of acid leach processing method of silvalin rope, which is characterized in that the silvalin rope is wound on creel, then
The creel for winding silvalin rope is placed in acid solution, and is rotated in acid solution, to realize that acid leach reacts.
2. the acid leach processing method of silvalin rope according to claim 1, which is characterized in that the section of the creel is
Regular polygon structure made of body of rod support, the silvalin rope are wound with winding than the requirement for 2-10, thickness no more than 3cm
In on the body of rod.
3. the acid leach processing method of silvalin rope as claimed in claim 2, which is characterized in that the section of the creel it is just more
The number of edges of side shape structure is 3-30.
4. the acid leach processing method of silvalin rope according to claim 2 or 3, which is characterized in that outside the creel
Connecing round radius is 15cm-1000cm.
5. the acid leach processing method of silvalin rope described in any one of -4 according to claim 1, which is characterized in that described turn
It is dynamic to refer to that the creel for being wound with silvalin rope is rotated around the central axis of creel, velocity of rotation 5-80rpm.
6. the acid leach processing method of silvalin rope according to any one of claims 1-5, which is characterized in that further include
The process of indirect heating is carried out to the acid solution.
7. the acid leach processing method of silvalin rope according to claim 1 to 6, which is characterized in that the acid
The equivalent concentration of liquid is 1.0-3.6N/L, and temperature is 80-100 DEG C, be wound with that the creel of silvalin rope rotates in acid solution when
Between be 60-150min.
8. the acid leach processing method of silvalin rope described in any one of -7 according to claim 1, which is characterized in that the fibre
Dimension yarn rope is alkali-free glass fibre yarn rope, Shift of Binary Sodium Silicate glass fiber yarn rope and tribasic sodium borosilicate fiberglass yarn rope
At least one of.
9. a kind of preparation method of high silica glass fiber yarns rope, which is characterized in that including any one of claim 1-10 institute
The acid leach processing method for the silvalin rope stated.
10. preparation method according to claim 9, which is characterized in that the acid leach processing before further include sour drip
Preprocessing process is filtered, in the acid leach preprocessing process, the equivalent concentration of acid solution is 1.4-3.6N/L, and temperature is 50-80 DEG C,
The processing time is 10-60min.
11. preparation method according to claim 9 or 10, which is characterized in that further include to acid leach treated fiber
Yarn rope carries out spray washing and soaking and water washing, until the pH value on silvalin rope surface is 6 or more.
12. preparation method according to claim 11, which is characterized in that the spray washing process are as follows: acid leach processing
After the completion, it maintains to carry out spray process to silvalin rope surface with water while creel rotation, to realize the process of spray washing.
13. preparation method according to claim 11 or 12, which is characterized in that the soaking and water washing process are as follows: maintain yarn
The creel for being wound with silvalin rope is dipped in the process that soaking and water washing is realized in water by frame rotation.
14. preparation method described in any one of 1-13 according to claim 1, which is characterized in that the spray washing and immersion
In water-washing process, the temperature of water is 60-80 DEG C, and the revolving speed of creel is 15-30rpm, wherein the number of spray washing is 2-4 times,
Each 5-10min, the number of soaking and water washing are 2-3 time, each 25-35min, and the spray washing and soaking and water washing replace into
Row.
15. the preparation method according to any one of claim 9-14, which is characterized in that further include at 100-150 DEG C
After removal washing process the step of the water of silvalin rope adsorption.
16. the preparation method according to any one of claim 9-15, which is characterized in that further include that single yarn rope is soaked in
In post-treatment agent, surface dipping process is carried out, is subsequently placed at 150-350 DEG C the step of drying film forming.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811344051.0A CN109371597A (en) | 2018-11-12 | 2018-11-12 | A kind of preparation method of acid leach processing method and high silica glass fiber yarns rope |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811344051.0A CN109371597A (en) | 2018-11-12 | 2018-11-12 | A kind of preparation method of acid leach processing method and high silica glass fiber yarns rope |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109371597A true CN109371597A (en) | 2019-02-22 |
Family
ID=65384979
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811344051.0A Pending CN109371597A (en) | 2018-11-12 | 2018-11-12 | A kind of preparation method of acid leach processing method and high silica glass fiber yarns rope |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109371597A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113846444A (en) * | 2021-09-23 | 2021-12-28 | 启东捷明密封科技有限公司 | Preparation method and system of high silica glass fiber rope with low heat conductivity coefficient |
| CN114477794A (en) * | 2022-03-02 | 2022-05-13 | 南京玻璃纤维研究设计院有限公司 | Heat setting device for glass fiber product |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2078703B (en) * | 1980-06-27 | 1983-06-08 | Steirische Magnesit Ind Ag | Producing active silica |
| CN101654836A (en) * | 2009-07-10 | 2010-02-24 | 江苏恒州特种玻璃纤维材料有限公司 | High silica glass fiber cloth and manufacturing process thereof |
| CN102320760A (en) * | 2011-07-15 | 2012-01-18 | 江苏恒州特种玻璃纤维材料有限公司 | A kind of equipment that is used for resurrection glass fibre yarn intermittent type acid leach treatment process |
| CN102864542A (en) * | 2012-09-09 | 2013-01-09 | 安徽省旌德县南关玻纤厂 | Process for manufacturing multielement composition high silica glass fibre fixed-length yarn |
| CN102863150A (en) * | 2012-09-25 | 2013-01-09 | 江苏恒州特种玻璃纤维材料有限公司 | Production technology for producing vitreous silica fiber short chopping yarns through cutting silks |
| CN105297313A (en) * | 2015-12-08 | 2016-02-03 | 常熟市耀星玻纤绝缘制品有限公司 | Acid leaching technology of high-silica glass fiber yarn |
| CN107354548A (en) * | 2017-07-15 | 2017-11-17 | 合肥皖水信息科技有限公司 | A kind of preparation method of high-strength high silica glass fiber yarns for fire smothering blanket |
| CN107651854A (en) * | 2017-10-24 | 2018-02-02 | 内江市旭日环境科技有限公司 | A kind of novel glass fiber |
-
2018
- 2018-11-12 CN CN201811344051.0A patent/CN109371597A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2078703B (en) * | 1980-06-27 | 1983-06-08 | Steirische Magnesit Ind Ag | Producing active silica |
| CN101654836A (en) * | 2009-07-10 | 2010-02-24 | 江苏恒州特种玻璃纤维材料有限公司 | High silica glass fiber cloth and manufacturing process thereof |
| CN102320760A (en) * | 2011-07-15 | 2012-01-18 | 江苏恒州特种玻璃纤维材料有限公司 | A kind of equipment that is used for resurrection glass fibre yarn intermittent type acid leach treatment process |
| CN102864542A (en) * | 2012-09-09 | 2013-01-09 | 安徽省旌德县南关玻纤厂 | Process for manufacturing multielement composition high silica glass fibre fixed-length yarn |
| CN102863150A (en) * | 2012-09-25 | 2013-01-09 | 江苏恒州特种玻璃纤维材料有限公司 | Production technology for producing vitreous silica fiber short chopping yarns through cutting silks |
| CN105297313A (en) * | 2015-12-08 | 2016-02-03 | 常熟市耀星玻纤绝缘制品有限公司 | Acid leaching technology of high-silica glass fiber yarn |
| CN107354548A (en) * | 2017-07-15 | 2017-11-17 | 合肥皖水信息科技有限公司 | A kind of preparation method of high-strength high silica glass fiber yarns for fire smothering blanket |
| CN107651854A (en) * | 2017-10-24 | 2018-02-02 | 内江市旭日环境科技有限公司 | A kind of novel glass fiber |
Non-Patent Citations (2)
| Title |
|---|
| 张耀明等: "《玻璃纤维与矿物棉全书》", 31 March 2001, 化学工业出版社 * |
| 徐国荣等: "《电化学设备与工程设计》", 31 March 2018, 中国矿业大学出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113846444A (en) * | 2021-09-23 | 2021-12-28 | 启东捷明密封科技有限公司 | Preparation method and system of high silica glass fiber rope with low heat conductivity coefficient |
| CN114477794A (en) * | 2022-03-02 | 2022-05-13 | 南京玻璃纤维研究设计院有限公司 | Heat setting device for glass fiber product |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109371597A (en) | A kind of preparation method of acid leach processing method and high silica glass fiber yarns rope | |
| CN102839476B (en) | Production process of high-strength high-silicon dioxide glass fiber yarns | |
| CN101654835B (en) | Thick high silica glass fiber cloth and manufacturing process thereof | |
| CN104787998B (en) | A kind of production technology of glass toughening manure pit | |
| CN107376509B (en) | The preparation method of the superfine modified glass fiber filter material of fluorine silicon oxygen | |
| CN101654834A (en) | High silica glass fiber mesh cloth and production technique thereof | |
| JP6841931B2 (en) | Bamboo fiber clean production | |
| CN101760858B (en) | Glass fiber strip with high silicon and oxygen content and manufacture process thereof | |
| CN101654836B (en) | Manufacturing process of high silica glass fiber cloth | |
| CN110644102A (en) | Processing technology of wear-resistant yarn | |
| CN107938315A (en) | A kind of protein modified method of polyester fabric | |
| CN103645082A (en) | Impregnation device and method for tensile property test of carbon fiber multifilaments | |
| CN113041863A (en) | Preparation method and application of defect-free and pollution-resistant zirconium-based metal organic framework film | |
| CN209636118U (en) | A kind of acid leach device of silvalin rope | |
| CN107869046A (en) | A kind of fibroin method of modifying of polyester fabric | |
| CN103787593A (en) | Preparation method for alkali-resistant fiberglass | |
| CN109678365A (en) | A kind of acid leach device of silvalin rope | |
| CN103898750A (en) | Sizing method of low-pollution textile slurry | |
| CN103882709A (en) | Sizing method of environment-friendly textile slurry | |
| CN102039984A (en) | Super-buoyancy superhydrophobic aramid fiber bundle ship and manufacturing method thereof | |
| CN102320760B (en) | Equipment used in intermittent acid leaching treatment process of high silica glass fiber yarns | |
| CN110004723B (en) | Preparation method of unidirectional perspiration fabric | |
| CN112553888B (en) | Zirconium carbide modified cloth and preparation method and application thereof | |
| CN209338718U (en) | Polyvinyl alcohol filament yarn prepares assembly line | |
| CN205636136U (en) | Super fine dyeing production line |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20200210 Address after: 210000 No.30, Andri, Yuhua West Road, Nanjing, Jiangsu Province Applicant after: NANJING FIBERGLASS RESEARCH & DESIGN INSTITUTE Co.,Ltd. Address before: 210000 Jiangsu city of Nanjing province Jiangning Science Park Tong Road No. 99 Applicant before: Sinoma Science & Technology Co.,Ltd. |
|
| TA01 | Transfer of patent application right | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190222 |
|
| RJ01 | Rejection of invention patent application after publication |