CN1156547C

CN1156547C - Technological process of producing bone gelatine for color photography

Info

Publication number: CN1156547C
Application number: CNB001059068A
Authority: CN
Inventors: 军王; 王军
Original assignee: DONGBAO LEKAI GELATINE Co Ltd BAOTOU
Current assignee: DONGBAO LEKAI GELATINE Co Ltd BAOTOU
Priority date: 2000-04-19
Filing date: 2000-04-19
Publication date: 2004-07-07
Anticipated expiration: 2020-04-19
Also published as: CN1318607A

Abstract

The present invention relates to a technological process for preparing gelatine for color photography from dry bones. The technological process is mainly characterized in that recovered waste and old dry bones are used, and the appearance color of gelatine for color photography is improved by new technologies, such as degreasing post-treatment, pickling post-treatment, water washing neutralization, resin adsorption, ultrafiltration, etc., and the physical and chemical indexes achieve the requirements by gelatine for color photography. The transmissivity of gelatine for color photography is improved by the technology, metallic impurities, such as copper, iron, etc., in the gelatine for color photography are reduced, and the gelatine for color photography can be used as gelatine for a color photosensitive material to take the place of imports.

Description

Process for producing colour photographic gelatin by using dry bone

The technical field is as follows:

the present invention relates to a technological process for producing photographic gelatin as main raw material for colour photosensitive material by using dry bone.

Secondly, background art:

the prior art adopts a soda ash method to obtain gelatin, and the process comprises the steps of material selection, crushing, degreasing, pickling, liming, neutralization, gelatin extraction, evaporation, drying, crushing, quality inspection and packaging, wherein the neutralization process is neutralization by hydrochloric acid for 5 times. The pigment carried by the hydrochloric acid directly influences the appearance of the gelatin, so the appearance and color of the produced product are poor; the transmittance is low: 450 nm: 70-75%, 620 nm: 80-85%; high copper and iron contents, Fe: 20PPm, Cu: 15 PPm; low freezing strength: bloom is 270g, so the intrinsic physical and chemical indexes of the product can not meet the requirements of color photographic gelatin.

Thirdly, the invention aims to:

the invention aims to provide the color photographic gelatin produced by using dry bones aiming at the defects in the prior art, the appearance and color of the color photographic gelatin are improved, the physicochemical indexes of the color photographic gelatin meet the requirements of the color photographic gelatin, and the level of producing the color photographic gelatin by using fresh bones abroad is reached.

Fourthly, the invention content:

the purpose of the invention is realized by adopting the following measures.

A process for producing colour photographic gelatin by using dry bone comprises the steps of selecting materials, crushing, hydraulic degreasing, degreasing post-treatment, pickling post-treatment, liming, water washing neutralization, gelatin extraction, resin adsorption, ultrafiltration, evaporation, drying, crushing, quality assurance and packaging, and is characterized in that: the physical and chemical indexes of the waste and old recovered dry bones meet the quality requirements of the color photographic gelatin by a new process method, wherein:

(1) post-degreasing treatment

Mixing the degreased aggregate with 0.5-1% sulfurous acid (H)₂SO₃) The aggregate is soaked in the solution for 48 hours to achieve the bleaching effect;

(2) post-pickling treatment

Washing ossein with water at pH not less than 5, adding 0.2% hydrogen peroxide (H)₂O₂) Solution, soaked for 24 hours, further bleached:

(3) water washing neutralization

Selecting different formulas according to different product requirements, wherein the formula comprises the following components in parts by weight:

a. controlling the viscosity to drop: washing with water for 16 hr, neutralizing with 0.2% hydrochloric acid (HCl) solution for two times (1 hr each time), adding 0.5% acetic acid solution for neutralization for 3 hr, draining off acid solution, washing with water for 36 hr, and packaging;

b. and (3) improving the transmittance: washing with water for 16 hours, neutralizing with 0.25% sulfuric acid for 5 hours, discharging acid liquor, washing with water for 36 hours, and fillinginto a pot;

c. improving the freezing force: washing with water for 16 hours, neutralizing with 0.2% phosphoric acid for three times, discharging acid liquor every 1 hour, washing with water for 36 hours, and filling into a pot;

(4) purification treatment process for glue solution after glue extraction

a. Resin adsorption: keeping the temperature of the glue solution at 50 ℃, sequentially passing through 4 resin columns connected in series, and sequentially passing through 4 resins of strong acid, strong base, weak acid and weak base, wherein:

resin filling ratio: strong acid to strong base to 1 to 2

Weak acid to weak base: 1: 2

Controlling the flow rate of the glue solution: less than 3000 l/h and less than 3000 l/h,

b. and (3) ultrafiltration: the temperature of the glue solution is kept at about 50 ℃ and the pressure is not more than 0.2 MPa.

Fifthly, the invention has the following effects:

the scale of domestic animal husbandry and slaughter industry is nearly hundreds of years different from that of domestic same industry, the domestic production of colour photographic gelatin mainly uses fresh ox bone as raw material, and the domestic production of gelatin mainly uses waste recovered dry bone, and can not be compared with domestic situation.

1. Photographic gelatin analysis report sheet (SC 19-75);

2. a raw material photographic performance identification report (original part name: Baotou glue No. 30);

3. a raw material photographic quality evaluation report (raw material name: standard);

4. the letter from the chinese le kai film group company to baotongbao le kai gelatin limited.

The novel process is mainly characterized in that:

1. light yellow in appearance and color

2. Transmittance: 450nm and more than 85 percent;

over 95% at 620 nm;

3. the content of copper and iron is low: fe: less than 5 PPm;

cu: less than 3 PPm;

4. freezing strength: bloom 300g or more.

Sixth, description of the accompanying drawings:

FIG. 1 is a process flow of the present invention;

seventhly, embodiment:

the following detailed description of the embodiments of the invention refers to the accompanying drawings:

1. sorting

According to the type and position (head, thigh and shin) of livestock, old bones and other impurities which are weathered and become black and yellow are sorted out.

The aggregate types are as follows: large head, large tube, small tube and mixed bone.

2. Crushing:

the sorted aggregate is finished by two working procedures of primary smashing and fine smashing.

The size range of the bone blocks after initial smashing is required: 20-45 mm;

the size range of the bone blocks after fine smashing requires: 5-25 mm.

3. Degreasing:

defatting is carried out in 10-15 min by using high temperature water (90-95 deg.C), low acidity (pH 5) and material-water ratio (1: 1). Then the oil water and the bone blocks are separated in a horizontal centrifuge. Drying the aggregate in a drier (with air temperature of 100 ℃ and drying time of 45-60 minutes) and then grading the aggregate according to the size and the specific gravity in a vibrating screen. The extra hard bone is used for producing photographic glue, and the hard bone is used as food glue and medicinal glue.

Bone oil is a by-product of this process.

4. Degreasing post-treatment:

defatting the aggregate with 0.5-1% sulfurous acid (H)₂SO₃) The solution is soaked for 48 hours to achieve the bleaching effect.

5. Pickling:

the bone pieces after degreasing, when pickled, undergo the following reactions:

the concentration of pickling is generally controlled at 5%, and is slightly changed according to different seasons.

Concentration in winter: 4.5-5.0%

Concentration in summer: 3.0 to 3.5 percent

Soaking at 20 deg.C for 7-8 days.

And (3) judging the pickling end point:

(1) after stirring by adding neo-acid, the pH changed slightly from 2 to 4.

(2) The thick portion of ossein is easily cut with a small knife and has elasticity when bent.

The mature ossein is washed to pH4-4.5 and awaited liming.

6. Pickling post-treatment:

washing ossein with water until pH is greater than or equal to 5, and adding 0.2% hydrogen peroxide (H)₂O₂) The solution is soaked for 24 hours and further bleached.

7. Liming:

lime milk is used as raw material after liming, the concentration of calcium oxide is 4%, the calcium oxide is properly increased in winter and is properly decreased in summer, and each batch of ossein needs to be soaked for about 50-80 days.

If the color of lime milk in the pool turns yellow or the PH is lower than 10, the lime should be changed immediately, and washing with water is carried out for 3 times each time the lime is changed.

Judging the end point of liming:

the isoelectric point of ossein was measured, and PI was 4.7 or so, which was regarded as an end point.

8. And (3) water washing neutralization:

different processes are selected according to different product requirements

The first process comprises the following steps: controlling the viscosity to drop:

washing with water for 16 h, neutralizing twice with 0.2% hydrochloric acid solution for 1 h, neutralizing with 0.5% acetic acid solution for 3 h, draining off acid solution, washing with water for 36 h, and loading into pot.

And a second process: and (3) improving the transmittance:

washing the ash with water for 16 hours, neutralizing with 0.25% sulfuric acid for 5 hours, discharging acid liquor, washing with water for 36 hours, and filling into a pot.

And a third process: improve the freezing power

And (3) removing ash, washing with water for 16 hours, neutralizing with 0.2% phosphoric acid for three times, discharging acid liquor after 1 hour each time, washing with water for 36 hours, and filling into a pot.

9. Extracting glue:

temperature, time and pH were controlled.

The extraction is generally divided into 5-6 times.

For the first time: 50-65 deg.C

And (3) for the second time: 65-70 deg.C

And thirdly: 70-75 deg.C

Fourth time: 75-85 deg.C

Fifth step: 90-95 deg.C

The gelatin extracted from the first three times can be used as photographic gelatin.

The pH value during extraction is controlled to be about 6.0, and the concentration of the extracted glue solution is about 6%.

10. Resin adsorption:

the temperature of the glue solution is kept at 50 ℃, and 4 resins of strong acid, strong base, weak acid and weak base are sequentially arranged on 4 resin columns which are connected in series. The main purposes are depigmentation, demetallization of impurities and non-collagenous proteins.

Resin filling ratio: strong acid to strong base to 1 to 2

Weak acid to weak base: 1: 2

Controlling the flow rate of the glue solution: less than 3000 l/h

11. And (3) ultrafiltration:

the temperature of the glue solution is kept at about 50 ℃ and the pressure is not more than 0.2 MPa.

12. And (3) evaporation:

vacuum evaporation is utilized, a three-effect vacuum evaporator is adopted, and the vacuum degree requires 450-500mm mercury.

The gum solution was concentrated to 25%.

13. And (3) drying:

the concentrated gelatin solution is processed into gel strips by a freezing and glue extruding machine, and then is conveyed into a long net dryer for drying, and about 70 percent of water is removed.

The drying process is divided into three drying zones: (T is temperature, RH is relative humidity)

A first drying area: t is 25 deg.C, RH is 42%

A second drying area: t is 35-40 deg.C, RH is 38%

A third drying area: t is 45-50 deg.C, RH is 38%

The final equilibration period allowed the dried gelatin to return to T30 ℃ and RH 42% for 4 hours for the entire drying process.

14. Crushing:

the dried gelatin is pulverized by a hammer mill.

15. Quality assurance inspection:

the crushed gelatin was sampled and assayed. The main indexes are as follows: viscosity, viscosity drop, clarity, pH.

16. Packaging:

and packaging according to the quality assurance test result, wherein 3-5 tons are used as a large batch number.

17. And (3) overall quality inspection:

and carrying out comprehensive analysis and assay on the packaged gelatin according to gelatin standards, and grading according to the achieved indexes.

18. And (3) storage:

the storehouse temperature is required to be below 20 ℃, and RH is about 50 percent, so the storehouse is clean and sanitary.

Eighthly, the invention has the advantages that: the method utilizes the waste recovered dry bone to achieve the physicochemicalindex of producing gelatin with foreign fresh bone through a new process method, thereby improving the appearance and color, improving the transmittance of the color photographic gelatin, and reducing metal impurities such as iron, copper and the like.

Claims

A process for preparing colour photographic gelatin from dried bone includes such steps as choosing raw materials, breaking, hydraulic defatting, post-treating after defatting, immersing in acid, post-treating after immersing in acid, immersing in ash, neutralizing by water washing, extracting gelatin, resin adsorption, ultrafiltering, evaporating, drying, pulverizing, quality assurance and packing, and features that: the physical and chemical indexes of the waste and old recovered dry bones meet the quality requirements of the color photographic gelatin by a new process method, wherein:

(1) post-degreasing treatment

Mixing the degreased aggregate with 0.5-1% sulfurous acid (H)₂SO₃) The aggregate is soaked in the solution for 48 hours to achieve the bleaching effect;

(2) post-pickling treatment

Washing ossein with water at pH not less than 5, adding 0.2% hydrogen peroxide (H)₂O₂) Solution, soaked for 24 hours, further bleached:

(3) water washing neutralization

Selecting different formulas according to different product requirements, wherein the formula comprises the following components in parts by weight:

a. controlling the viscosity to drop: washing with water for 16 hr, neutralizing with 0.2% hydrochloric acid (HCl) solution for two times (1 hr each time), adding 0.5% acetic acid solution for neutralization for 3 hr, draining off acid solution, washingwith water for 36 hr, and packaging;

b. and (3) improving the transmittance: washing with water for 16 hours, neutralizing with 0.25% sulfuric acid for 5 hours, discharging acid liquor, washing with water for 36 hours, and filling into a pot;

c. improving the freezing force: washing with water for 16 hours, neutralizing with 0.2% phosphoric acid for three times, discharging acid liquor every 1 hour, washing with water for 36 hours, and filling into a pot;

(4) purification treatment process for glue solution after glue extraction

a. Resin adsorption: keeping the glue solution at 50 ℃, sequentially passing through 4 resin columns connected in series, and sequentially passing through 4 resins of strong acid, strong base, weak acid and weak base, wherein:

resin filling ratio side: strong acid to strong base to 1 to 2

Weak acid to weak base: 1: 2

Controlling the flow rate of the glue solution: less than 3000 liters/hour;

b. and (3) ultrafiltration: the temperature of the glue solution is kept at about 50 ℃ and the pressure is not more than 0.2 MPa.