CN107523890A - A kind of preparation method of the super-fine fiber material of anti-neutron irradiation - Google Patents
A kind of preparation method of the super-fine fiber material of anti-neutron irradiation Download PDFInfo
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- CN107523890A CN107523890A CN201710798582.6A CN201710798582A CN107523890A CN 107523890 A CN107523890 A CN 107523890A CN 201710798582 A CN201710798582 A CN 201710798582A CN 107523890 A CN107523890 A CN 107523890A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/06—Feeding liquid to the spinning head
- D01D1/09—Control of pressure, temperature or feeding rate
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/10—Filtering or de-aerating the spinning solution or melt
- D01D1/106—Filtering
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
- D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
Abstract
The invention provides a kind of preparation method of the super-fine fiber material of anti-neutron irradiation, and the super-fine fiber material is with PP sections and nanometer B4C blends are raw material, and titanate coupling agent and TAS 2A are additive, using meltblown by PP/B4C blend melt spinnings.The present invention is by Moderation of the fast neutrons material（Polypropylene）With slow neutron absorbing material（Nano boron carbide）Both blendings, on the basis of being modified using titanate coupling agent to nano silicon carbide boron surface, with the addition of TAS 2A dispersants, make a nanometer B again4C is equably attached on carrier surface, and PP/B is made4It is blended in proportion with matrix section after C master batches, using meltblown melt spinning, nano boron carbide is set to be dispersed in polypropylene superfine fiber, obtained superfine fibre Web materials are soft, fluffy, frivolous, good permeability, and then are made to protective garment of the thermal neutron protective shielding rate up to 80%.
Description
Technical field
The invention belongs to spinning field, and in particular to a kind of preparation method of the super-fine fiber material of anti-neutron irradiation.
Background technology
Neutron is a kind of uncharged neutral particle, has point of fast neutron and slow neutron, its penetration power is very strong, in air
Farther out, there are some researches show harm of the neutron to human body is significantly larger than X ray and gamma-rays for middle propagation distance.NEUTRON PROTECTION essence is just
It is by Moderation of the fast neutrons and slow neutron absorption, and then by neutron shield.
Boron-containing compound is the optimal shielding material for preparing neutron radiation protection material, and domestic and international NEUTRON PROTECTION material more will
Hydrogeneous more high polymer and composite board is made for inorganic boride melt blending or spinning is made into clothes again.Polypropylene（PP）And carbon
Change boron（B4C）It is conventional NEUTRON PROTECTION material, boron carbide uniformly must just be avoided that radiation shield by interspersed high in polypropylene
The perforation effect covered, but chemically inert B4C and non-polar compound PP compatibility are very poor, so relevant PP/B4C
The Study on Compatibility of co-mixing system is a big key issue of anti-neutron irradiation material development.
At present using in B4Coupling agent is added in C and PP blend（Silane coupler, titanate coupling agent）Come to B4C
Surface is modified, so as to improve B4C wellability, dispersiveness, but pass through electron microscopic observation, B4C particle aggregation phenomenons are serious, nothing
Method is really realized dispersed.Therefore, in order to improve neutron shield rate, B can only be increased4C content（Boron carbide sheath core fiber is most
Big content 40%, the addition of composite board are higher）With composite board, fabric thickness, fabric will be made soft during as dress materials
Soft difference, gas permeability is bad, excessively heavy, handicapped, expensive, and protects leak more, does not reach requirement of shelter
Index.
The content of the invention
The present invention is to solve prior art and the above mentioned problem present in raw material, there is provided a kind of physical and chemical performance is excellent
PP/B good, that neutron shield is functional and frivolous, soft4The preparation method of C superfine fibre Web materials.
NEUTRON PROTECTION is substantially exactly by Moderation of the fast neutrons and slow neutron absorption and then by neutron shield.The material of Moderation of the fast neutrons
Material mainly has the very high paraffin of protium content, polyethylene and polypropylene etc.；The material that slow neutron absorbs mainly has containing elemental lithium
Lithium fluoride, lithium bromide, lithium hydroxide, boron oxide, boron carbide and rare earth element containing boron element.
Realize the technical scheme is that：A kind of preparation method of the super-fine fiber material of anti-neutron irradiation is described super
Fine fiber material is with PP sections and nanometer B4C blends are raw material, and titanate coupling agent and TAS-2A are additive, using melt-blown
Method is by PP/B4C blend melt spinnings.
Comprise the following steps that：
（1）PP/B4The preparation of C master batches：First PP is cut into slices, titanate coupling agent is mixed in high-speed kneading machine, work as temperature
By nanometer B when reaching 90 DEG C4C and TAS-2A is added, and discharging cooling after 20-30min is mixed, with double screw extruder melting extrusion
It is granulated, obtains PP/B4C master batches；
（2）To step（1）Obtained PP/B4C master batches are dried, 100-120 DEG C of drying temperature, drying time 2-3h；
（3）By step（2）Dried PP/B4C master batches and PP sections are using mass ratio as 1:Screw extruder is sent into after 2 mixing,
Melt-spraying spinning component is delivered to after screw rod melting extrusion, filter filtering, metering pump-metered, melt passes through after spinneret orifice is extruded
Superfine fibre is generated after air drawing, superfine fibre into collection on lace curtaining through forming super-fine fiber material.
The step（1）Middle PP sections, nanometer B4C, titanate coupling agent and TAS-2A mass ratio are（70-90）：
（10-20）：（3-8）：（1.5-3）.
The step（1）The temperature that middle double screw extruder melting extrusion is granulated is：I 160 DEG C of area, 170 DEG C of IIth area, IIIth area
170 DEG C, 172 DEG C of IVth area, 162 DEG C of head.
The step（2）PP/B after middle drying4C master batch water content controls are in below 800ppm.
The step（3）Each area's temperature of middle screw extruder is 175-245 DEG C, 240-250 DEG C of filter temperature, metal
Screen pack mesh number is 300 mesh；235-250 DEG C of the temperature of measuring pump, 235-250 DEG C of the spinning die head temperature of melt-spraying spinning component；
The drawing-off blast of air drawing step is 2-4bar, and drawing-off air temperature is 240-250 DEG C；The absorption negative pressure of networking step is 0.3-
0.4bar, it is 200-300mm into the distance between lace curtaining and die head spinneret.
The step（1）The performance parameter of middle PP section is：167 DEG C of fusing point, melt mass flow rate are born at 260 DEG C
40-60g/10min is reached under conditions of weight 2160g, relative molecular mass distribution width is less than 4-5.
The step（3）The performance parameter of middle PP section is：167 DEG C of fusing point, melt mass flow rate are born at 260 DEG C
800-1500g/10min is reached under conditions of weight 2160g, relative molecular mass distribution width is less than 4-5.
The nanometer B4C average grain diameters are 60nm.
The string diameter of the super-fine fiber material is 0.5-30 μm, and because fibre diameter is small, face coverage rate is high, therefore B4C exists
It is evenly distributed in whole web, so as to reach less B4C additions, higher neutron-absorbing effect.
The beneficial effects of the invention are as follows：By Moderation of the fast neutrons material（Polypropylene）With slow neutron absorbing material（Boron carbide）Two
Person is blended, and on the basis of being modified using titanate coupling agent to carbonization boron surface, with the addition of TAS-2A dispersants again, makes nanometer
B4C is equably attached on carrier surface, and PP/B is made4Melt finger PP sections with height after C master batches to be blended in proportion, melted using meltblown
Melt spinning, nano boron carbide is dispersed in polypropylene superfine fiber, obtained superfine fibre Web materials are soft, fluffy
Loose, frivolous, good permeability, and then be made to protective garment of the thermal neutron protective shielding rate up to 80%.Pretective acreage is big, shields neutron
Line ability is strong, in light weight, and thickness is moderate, is easy to wear off, soft comfortable, breathable insulation, unleaded, without rubber, no thermoset elastic
Body.Be widely used in oil well logging, geological prospecting, coal industry, instrument calibration room, ordnance missile maintenance, reactor building,
Nuclear fuel material refinery, tank, panzer occupant, national defence naval vessel builds the nuclear defence of personnel and chemical defense force officers and men and neutron is prevented
Shield, road construction neutron measurement scene, the medical worker near neutron knife and patient's protection etc..
Brief description of the drawings
Fig. 1 is the dsc analysis figure for the PP that the present invention uses.
Fig. 2 is the nanometer B that the present invention uses4C electron microscope.
Fig. 3 is nanometer B under petrographic microscope4C is in PP/B4Deployment conditions in C master batches.
Fig. 4 is nanometer B under petrographic microscope4Deployment conditions of the C in superfine fibre.
Embodiment
Embodiment 1
The preparation method of the super-fine fiber material of the anti-neutron irradiation of the present embodiment, step are as follows：
The super-fine fiber material is with PP sections and nanometer B4C blends are raw material, and titanate coupling agent and TAS-2A are addition
Agent, using meltblown by PP/B4C blend melt spinnings, the nanometer B4C average grain diameters are in 60nm or so.
The preparation method of the super-fine fiber material of described anti-neutron irradiation, is comprised the following steps that：
（1）PP/B4The preparation of C master batches：First PP is cut into slices, titanate coupling agent is mixed in high-speed kneading machine, PP sections
Performance parameter be：167 DEG C of fusing point, PP sections, which are melted, under conditions of 260 DEG C of heavy burden 2160g, in master batch refers to 56g/10min, when
By nanometer B when temperature reaches 90 DEG C4C and TAS-2A is added, and is mixed discharging cooling after 20min, is melted and squeezed with double screw extruder
Go out to be granulated, obtain PP/B4C master batches；Double screw extruder melting extrusion be granulated temperature be：I 160 DEG C of area, 170 DEG C of IIth area, III
170 DEG C of area, 172 DEG C of IVth area, 162 DEG C of head；PP sections, nanometer B4C, titanate coupling agent and TAS-2A mass ratio are 70：
10：3：1.5；
（2）To step（1）Obtained PP/B4C master batches are dried, 110 DEG C, drying time 2.5h of drying temperature, PP/ after drying
B4C master batch water content controls are in below 800ppm；
（3）By step（2）Dried PP/B4C master batches are pressed with PP chipping qualities than 1:Screw extruder, PP are sent into after 2 mixing
Section melts finger as 1000g/10min or so, and by screw rod melting extrusion, each area's temperature of screw extruder is 175-245 DEG C, mistake
Filter filters：240 DEG C of filter temperature, metal filter screen mesh number are 300 mesh；Melt-spraying spinning component is delivered to after metering pump-metered,
235 DEG C of the temperature of measuring pump, 235 DEG C of the spinning die head temperature of melt-spraying spinning component；Melt is led after spinneret orifice is extruded through air-flow
Superfine fibre is generated after stretching, the drawing-off blast of air drawing step is 2bar, and drawing-off air temperature is 240 DEG C；Superfine fibre through into
Collected on lace curtaining and form super-fine fiber material, the absorption negative pressure of networking step is 0.3bar, between lace curtaining and die head spinneret
Distance is 200mm, and the string diameter of the fine fiber material is 0.5-30 μm.
Embodiment 2
The present embodiment provides a kind of preparation method of the super-fine fiber material of anti-neutron irradiation, and step is as follows：
The super-fine fiber material is with PP sections and nanometer B4C blends are raw material, and titanate coupling agent and TAS-2A are addition
Agent, using meltblown by PP/B4C blend melt spinnings, the nanometer B4C average grain diameters are in 60nm or so.
The preparation method of the super-fine fiber material of described anti-neutron irradiation, is comprised the following steps that：
（1）PP/B4The preparation of C master batches：First PP is cut into slices, titanate coupling agent is mixed in high-speed kneading machine, PP sections
Performance parameter be：167 DEG C of fusing point, PP sections, which are melted, under conditions of 260 DEG C of heavy burden 2160g, in master batch refers in 40g/10min,
Relative molecular mass distribution width is less than 4-5, when temperature reaches 90 DEG C by nanometer B4C and TAS-2A is added, after mixing 25min
Discharging cooling, is granulated with double screw extruder melting extrusion, obtains PP/B4C master batches；What double screw extruder melting extrusion was granulated
Temperature is：I 160 DEG C of area, 170 DEG C of IIth area, 170 DEG C of IIIth area, 172 DEG C of IVth area, 162 DEG C of head；PP sections, nanometer B4C, titanate esters
Coupling agent and TAS-2A mass ratio are 80：15：5：2.
（2）To step（1）Obtained PP/B4C master batches are dried, 100 DEG C, drying time 3h of drying temperature, after drying
PP/B4C master batch water content controls are in below 800ppm；
（3）By step（2）Dried PP/B4C master batches are pressed with PP chipping qualities than 1:Screw extruder, PP are sent into after 2 mixing
The performance parameter of section is：167 DEG C of fusing point, melt mass flow rate reach 800g/ under conditions of 260 DEG C, heavy burden 2160g
10min, relative molecular mass distribution width is less than 4-5, and by screw rod melting extrusion, each area's temperature of screw extruder is 175-
245 DEG C, filter filtering：245 DEG C of filter temperature, metal filter screen mesh number are 300 mesh；Melt-blown is delivered to after metering pump-metered to spin
Silk component, 245 DEG C of the temperature of measuring pump, 245 DEG C of the spinning die head temperature of melt-spraying spinning component；Melt passes through after spinneret orifice is extruded
Superfine fibre is generated after air drawing, the drawing-off blast of air drawing step is 3bar, and drawing-off air temperature is 245 DEG C；Ultra-fine fibre
Dimension into collection on lace curtaining through forming super-fine fiber material, and the absorption negative pressure of networking step is 0.35bar, into lace curtaining and die head spinneret
Distance between plate is 250mm.The string diameter of the fine fiber material is 0.5-30 μm.
The test of the present embodiment light transmittance uses spectrophotometer, transmitted light flux/incident flux of light transmittance=sample.
Sample grammes per square metre 70g/m2, thickness 0.55mm.It the results are shown in Table 1.
Table 1 is using spectrophotometer to 1 ~ 7 layer of PP/B4C superfine fibres net carries out light transmittance test value.
| The number of plies | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| Light transmittance | 0.1334 | 0.0202 | 0.0056 | 0.0030 | 0.0020 | 0.0020 | 0.0020 |
Embodiment 3
The present embodiment provides a kind of preparation method of the super-fine fiber material of anti-neutron irradiation, and step is as follows：
The super-fine fiber material is with PP sections and nanometer B4C blends are raw material, and titanate coupling agent and TAS-2A are addition
Agent, using meltblown by PP/B4C blend melt spinnings, the nanometer B4C average grain diameters are in 60nm or so.
The preparation method of the super-fine fiber material of described anti-neutron irradiation, is comprised the following steps that：
（1）PP/B4The preparation of C master batches：First PP is cut into slices, titanate coupling agent is mixed in high-speed kneading machine, PP sections
Performance parameter be：167 DEG C of fusing point, PP sections, which are melted, under conditions of 260 DEG C of heavy burden 2160g, in master batch refers in 60g/10min,
When temperature reaches 90 DEG C by nanometer B4C and TAS-2A is added, and is mixed discharging cooling after 20-30min, is melted with double screw extruder
Melt extruding pelletization, obtain PP/B4C master batches；Double screw extruder melting extrusion be granulated temperature be：I 160 DEG C of area, II area 170
DEG C, 170 DEG C of IIIth area, 172 DEG C of IVth area, 162 DEG C of head；PP sections, nanometer B4C, titanate coupling agent and TAS-2A mass ratio
For 90：20：8：3.
（2）To step（1）Obtained PP/B4C master batches are dried, 120 DEG C, drying time 2h of drying temperature, after drying
PP/B4C master batch water content controls are in below 800ppm；
（3）By step（2）Dried PP/B4C master batches are pressed with PP chipping qualities than 1:Screw extruder, PP are sent into after 2 mixing
It is 900g/10min that finger is melted in section, and by screw rod melting extrusion, each area's temperature of screw extruder is 175-245 DEG C, filter
Filtering：250 DEG C of filter temperature, metal filter screen mesh number are 300 mesh；Melt-spraying spinning component is delivered to after metering pump-metered, is measured
250 DEG C of the temperature of pump, 250 DEG C of the spinning die head temperature of melt-spraying spinning component；Melt is after spinneret orifice is extruded after air drawing
Superfine fibre is generated, the drawing-off blast of air drawing step is 4bar, and drawing-off air temperature is 250 DEG C；Superfine fibre is through into lace curtaining
Upper collection forms super-fine fiber material, and the absorption negative pressure of networking step is 0.4bar, the distance between lace curtaining and die head spinneret
For 300mm.The string diameter of the fine fiber material is 0.5-30 μm.
Claims (10)
1. a kind of preparation method of the super-fine fiber material of anti-neutron irradiation, it is characterised in that step is as follows：The superfine fibre
Material is with PP sections and nanometer B4C blends are raw material, and titanate coupling agent and TAS-2A are additive, will using meltblown
PP/B4C blend melt spinnings.
2. the preparation method of the super-fine fiber material of anti-neutron irradiation according to claim 1, it is characterised in that specific step
It is rapid as follows：
（1）PP/B4The preparation of C master batches：First PP is cut into slices, titanate coupling agent is mixed in high-speed kneading machine, when temperature reaches
To at 90 DEG C by nanometer B4C and TAS-2A is added, and is mixed discharging cooling after 20-30min, is made with double screw extruder melting extrusion
Grain, obtains PP/B4C master batches；
（2）To step（1）Obtained PP/B4C master batches are dried, 100-120 DEG C of drying temperature, drying time 2-3h；
（3）By step（2）Dried PP/B4C master batches and PP sections are using mass ratio as 1:Screw extruder is sent into after 2 mixing, is passed through
Melt-spraying spinning component is delivered to after crossing screw rod melting extrusion, filter filtering, metering pump-metered, melt is after spinneret orifice is extruded through gas
Drawing-off generation superfine fibre is flowed, superfine fibre into collection on lace curtaining through forming super-fine fiber material.
3. the preparation method of the super-fine fiber material of anti-neutron irradiation according to claim 2, it is characterised in that：The step
Suddenly（1）Middle PP sections, nanometer B4C, titanate coupling agent and TAS-2A mass ratio are（70-90）：（10-20）：（3-8）：
（1.5-3）.
4. the preparation method of the super-fine fiber material of anti-neutron irradiation according to claim 2, it is characterised in that：The step
Suddenly（1）The temperature that middle double screw extruder melting extrusion is granulated is：I 160 DEG C of area, 170 DEG C of IIth area, 170 DEG C of IIIth area, IV area 172
DEG C, 162 DEG C of head.
5. the preparation method of the super-fine fiber material of anti-neutron irradiation according to claim 2, it is characterised in that：The step
Suddenly（2）PP/B after middle drying4C master batch water content controls are in below 800ppm.
6. the preparation method of the super-fine fiber material of anti-neutron irradiation according to claim 2, it is characterised in that：The step
Suddenly（3）Each area's temperature of middle screw extruder is 175-245 DEG C, 240-250 DEG C of filter temperature, and metal filter screen mesh number is
300 mesh；235-250 DEG C of the temperature of measuring pump, 235-250 DEG C of the spinning die head temperature of melt-spraying spinning component；Air drawing step
Drawing-off blast be 2-4bar, drawing-off air temperature is 240-250 DEG C；The absorption negative pressure of networking step is 0.3-0.4bar, networking
Distance between curtain and die head spinneret is 200-300mm.
7. the preparation method of the super-fine fiber material of the anti-neutron irradiation according to claim 1-6, it is characterised in that：It is described
Step（1）The performance parameter of middle PP section is：167 DEG C of fusing point, melt mass flow rate is at 260 DEG C, heavy burden 2160g condition
40-60g/10min is assigned, relative molecular mass distribution width is less than 4-5.
8. the preparation method of the super-fine fiber material of the anti-neutron irradiation according to claim 1-6, it is characterised in that：It is described
Step（3）The performance parameter of middle PP section is：167 DEG C of fusing point, melt mass flow rate is at 260 DEG C, heavy burden 2160g condition
800-1000g/10min is assigned, relative molecular mass distribution width is less than 4-5.
9. the preparation method of the super-fine fiber material of the anti-neutron irradiation according to claim 1-6, it is characterised in that：It is described
Nanometer B4C average grain diameters are 60nm.
10. the preparation method of the super-fine fiber material of the anti-neutron irradiation according to claim 1-6, it is characterised in that：Institute
The string diameter for stating fine fiber material is 0.5-30 μm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110735208A (en) * | 2019-09-03 | 2020-01-31 | 刘禹超 | Industrial production method of neutron radiation protection fiber materials |
| CN115926216A (en) * | 2022-08-24 | 2023-04-07 | 西安工程大学 | Preparation method of flexible neutron composite shielding body based on metal hydride |
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