CN108948228A - A kind of method that spray drying prepares Phosphation agar - Google Patents

A kind of method that spray drying prepares Phosphation agar Download PDF

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Publication number
CN108948228A
CN108948228A CN201810649172.XA CN201810649172A CN108948228A CN 108948228 A CN108948228 A CN 108948228A CN 201810649172 A CN201810649172 A CN 201810649172A CN 108948228 A CN108948228 A CN 108948228A
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Prior art keywords
agar
spray drying
phosphation
solution
added
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CN201810649172.XA
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Inventor
钟晓婷
肖安风
嵇海峰
翁惠芬
洪清林
肖琼
郭东旭
洪菲菲
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FUJIAN PROVINCE LVQI FOOD COLLOID Co Ltd
Jimei University
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FUJIAN PROVINCE LVQI FOOD COLLOID Co Ltd
Jimei University
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Priority to CN201810649172.XA priority Critical patent/CN108948228A/en
Publication of CN108948228A publication Critical patent/CN108948228A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Molecular Biology (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Medicinal Preparation (AREA)
  • Edible Seaweed (AREA)
  • Jellies, Jams, And Syrups (AREA)

Abstract

The invention belongs to agar processing technique fields, and in particular to a kind of method that spray drying prepares Phosphation agar.Include the following steps: that agar powder is appropriate, a certain proportion of distilled water is added, then a certain proportion of phosphate ester agent is added in stirring, proper catalyst is added, and after the dissolution completely of all reagents, adjusts pH value, finally spray-dried to obtain modified agar powder.This method simple process, easily operated, the period is shorter, and agents useful for same is safe and non-toxic, products obtained therefrom is best in quality, has gel strength high, viscosity is low, and molten point is low, the advantages that transparency is good increases the type of agar, opens the new application field of agar, has preferable industrialization value.

Description

A kind of method that spray drying prepares Phosphation agar
Technical field
The present invention relates to the sides that agar processing technique field more particularly to a kind of spray drying prepare Phosphation agar Method.
Background technique
Agar is a kind of natural polysaccharide extracted from red algae seaweed, is that purposes is most widely extra large in the world at present
One of phycocolloid.Agar has excellent gelling and gel stability, is widely used in food, medicine, daily-use chemical industry, biology Many aspects such as engineering.Agar passes through the agarose that processing obtains, and is a kind of excellent Immune proliferation medium, is widely used in facing Bed, biochemical, immunology analysis and research.
Modified agar is by either physically or chemically, making the performance of agar change, to reach what agar was modified Purpose.Physical method mainly has microwave, radiation, ultrasonic wave etc..Chemical method, which refers to, connects new group on former agar molecule, Its property is set to change.The modified agar of reported chemical method mainly has using the modified oxidation agar of hydrogen peroxide, peroxide The hydroxypropyl agar of carboxymethyl agar, epoxy pronane modification that change hydrogen and trichloroacetic acid are modified is prepared by introducing acetyl group Arrive acetate agar etc..Compared with former agar, modified agar is in gel strength, solution temperature, melt temperature, gel temperature Degree, thermal stability, viscosity etc. have different degrees of variation.Different performances assigns agar different applications, and therefore, modification is Increase agar type, expands the preferable channel of agar application range.
About Phosphation agar, there has been no document reports at present.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of Phosphation agar, are tried using safe and non-toxic chemistry Agent, by the pyroreaction in spray drying tower, so that it is good to prepare low viscosity, low melting point, high-gel strength, transparency Modification agar, increase the type of agar, expand the application field of agar.This method simple process, easily controllable, product Production cycle is shorter, materials safety and source is wide, and product has higher application value.
To achieve the goals above, the technical solution adopted by the present invention is as follows:
A kind of method that spray drying prepares Phosphation agar, includes the following steps:
Step 1: weighing appropriate agar powder, adds water by the mass ratio of 1:10 ~ 1:30, be stirred continuously under room temperature;
Step 2: weighing a certain amount of mixed phosphate, it is added in agar solution;
Step 3: weighing a certain amount of catalyst, it is added with stirring in agar solution, until being completely dissolved;
Step 4: adjusting solution ph 5 ~ 7 after the reagent in solution is completely dissolved;
Step 5: under stiring, agar powder solution being sent into spray drying tower with certain flow rate and is sprayed;
Step 6: sieving, collects powder.
As the preferred embodiment of embodiment, in above-mentioned steps one, the material-water ratio of agar powder and water is 1:20;
As the preferred embodiment of embodiment, in above-mentioned steps two, the adding proportion of mixed phosphate be agar powder quality 25 ~ 30%;
As the preferred embodiment of embodiment, in above-mentioned steps three, the additive amount of used catalyst is the 5% of agar powder quality;
As the preferred embodiment of embodiment, in above-mentioned steps four, solution ph 5;
As the preferred embodiment of embodiment, in above-mentioned steps five, the flow velocity of agar solution is 9 rpm, the charging of spray drying tower Temperature is 150 ~ 155 DEG C, and atomisation pressure is 0.2 MPa.
Remarkable advantage of the invention:
The present invention is after adopting the above technical scheme, add water to mix agar powder raw material and mixed phosphate, by chemically and physically In conjunction with method, obtain modified agar, resulting agar has different degrees of variation in the performances such as molten point, viscosity, transparency, And it ensure that the gel strength of agar to the maximum extent.This method simple process, the period is short, and agents useful for same is safe and non-toxic, is suitable for Industrialization production.
Detailed description of the invention
Fig. 1 agar raw material, agar spraying (comparative example), the infrared spectrogram of Phosphation agar;Wherein A curve is fine jade Fat raw material;B curve is spraying for agar;C curve is Phosphation agar.
Specific embodiment
Embodiment 1
Step 1: weighing agar powder 10g, add water by the mass ratio of 1:15, stirs;
Step 2: weighing sodium dihydrogen phosphate 1.7g, disodium hydrogen phosphate 1.3g is added in agar solution, stirring;
Step 3: weighing urea 0.5g, it is added with stirring in agar solution, stirs;
Step 4: adjusting solution ph 5 after the reagent in solution is completely dissolved;
Step 5: setting spray drying tower operating parameter: 150 DEG C of feeding temperature, atomisation pressure 0.2MPa;
Step 6: being kept stirring state, 10 rpm of wriggling flow rate pump is adjusted, agar powder solution is sent into spray drying tower and is carried out It is spraying;
Step 7: sieving, collects powder.
Agar powder obtained by the present embodiment, through detecting, 85.7 DEG C of molten point, viscosity is 7.0 mPa s, gel strength 977 g/cm2, 68.1 % of transparency, agar powder yield is 48.8%.
Embodiment 2
Step 1: weighing agar powder 30g, add water by the mass ratio of 1:20, stirs;
Step 2: weighing sodium dihydrogen phosphate 5.1g, disodium hydrogen phosphate 3.9g is added in agar solution, stirring;
Step 3: weighing urea 1.5g, it is added with stirring in agar solution, stirs;
Step 4: adjusting solution ph 5 after the reagent in solution is completely dissolved;
Step 5: setting spray drying tower operating parameter: 155 DEG C of feeding temperature, atomisation pressure 0.2MPa;
Step 6: being kept stirring state, 9 rpm of wriggling flow rate pump is adjusted, agar powder solution is sent into spray drying tower and is carried out It is spraying;
Step 7: sieving, collects powder.
Agar powder obtained by the present embodiment, through detecting, 84.7 DEG C of molten point, viscosity is 6.5 mPa s, gel strength 947 g/cm2, 67.9 % of transparency, agar powder yield is 53.8%.
Embodiment 3
Step 1: weighing agar powder 50g, add water by the mass ratio of 1:20, stirs;
Step 2: weighing 8.5 g of sodium dihydrogen phosphate, 6.5 g of disodium hydrogen phosphate is added in agar solution, stirring;
Step 3: weighing urea 2.5g, it is added with stirring in agar solution, stirs;
Step 4: adjusting solution ph 5 after the reagent in solution is completely dissolved;
Step 5: setting spray drying tower operating parameter: 155 DEG C of feeding temperature, atomisation pressure 0.2MPa;
Step 6: be kept stirring state, adjust 8.5 rpm of wriggling flow rate pump, by agar powder solution be sent into spray drying tower into Row is spraying;
Step 7: sieving, collects powder.
Agar powder obtained by the present embodiment, through detecting, 84.3 DEG C of molten point, viscosity is 6.0 mPa s, gel strength 936 g/cm2, 69.5 % of transparency, agar powder yield is 56.5%.
Embodiment 4
Step 1: weighing agar powder 100g, add water by the mass ratio of 1:20, stirs;
Step 2: weighing 17.0 g of sodium dihydrogen phosphate, 13.0 g of disodium hydrogen phosphate is added in agar solution, stirring;
Step 3: weighing urea 5.0g, it is added with stirring in agar solution, stirs;
Step 4: adjusting solution ph 5 ~ 5.5 after the reagent in solution is completely dissolved;
Step 5: setting spray drying tower operating parameter: 155 DEG C of feeding temperature, 0.15 ~ 0.2 MPa of atomisation pressure;
Step 6: be kept stirring state, adjust 8.5 rpm of wriggling flow rate pump, by agar powder solution be sent into spray drying tower into Row is spraying;
Step 7: sieving, collects powder.
Agar powder obtained by the present embodiment, through detecting, 86.2 DEG C of molten point, viscosity is 7.2 mPa s, gel strength 986 g/cm2, 69.2 % of transparency, agar powder yield is 55.5%.
Comparative example
Step 1: weighing 10g agar powder, add water by the mass ratio of 1:20, stir, adjusts solution ph 5;
Step 2: setting spray drying tower operating parameter: 155 DEG C of feeding temperature, atomisation pressure 0.2MPa;
Step 3: being kept stirring state, 9 rpm of wriggling flow rate pump is adjusted, agar powder solution is sent into spray drying tower and is carried out It is spraying;
Step 4: sieving, collects powder.
Agar powder obtained by the present embodiment, through detecting, 92.2 DEG C of molten point, viscosity is 11.5 mPa s, gel strength 1145 g/cm2, 60.1 % of transparency, agar powder yield is 52.1%.
Each embodiment main indicator parameter of table 1
As can be seen from Table 1, the agar powder in embodiment 1 ~ 4 compares with raw material and comparative example, and gel strength has no significantly Difference, and viscosity and molten point are then decreased obviously, and transparency improves.It follows that being prepared by spray drying process Obtained Phosphation agar has higher product quality.
As seen from Figure 1, Phosphation agar is in 1300 ~ 1400cm-1There are two new peak (red circle marks in place At note), illustrate agar after esterification, chemical structure is changed.It is advised according to the vibration of fatty phosphorus compound group Rule, the stretching vibration absorption band of phosphoryl P=O, position distribution is very wide in the compound of different structure, can 1400 ~ 1150cm-1Between occur, it is understood that the peak occurred in Fig. 1 be P=O stretching vibration caused by.
The present invention is using chemically and physically combining, using safe and non-toxic mixed phosphate as esterifying agent, by doing by spraying Phosphation agar is prepared in dry method, in the case where not influencing gel strength, significantly reduces the molten point and viscosity of agar, And the transparency of agar is improved to a certain extent, product quality is improved, agar type is increased, is opened up for the application of agar Frontier, has certain industrialization value.
Above embodiments are merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.The common skill of this field All deformations that art personnel directly can export or associate from the disclosure of invention, are considered as protection model of the invention It encloses.

Claims (8)

1. a kind of method that spray drying prepares Phosphation agar, which comprises the steps of:
Step 1: weighing appropriate agar powder, adds water by the mass ratio of 1:10 ~ 1:30, be stirred continuously under room temperature;
Step 2: weighing a certain amount of mixed phosphate, it is added in agar solution;
Step 3: weighing a certain amount of catalyst, it is added with stirring in agar solution, until being completely dissolved;
Step 4: adjusting solution ph 5 ~ 7 after the reagent in solution is completely dissolved;
Step 5: under stiring, agar powder solution being sent into spray drying tower with certain flow rate and is sprayed;
Step 6: sieving, collects powder.
2. the method that a kind of spray drying prepares Phosphation agar according to claim 1, it is characterised in that: step In one, in agar powder solution, solid-liquid ratio is 1:20 ~ 1:25.
3. the method that a kind of spray drying prepares Phosphation agar according to claim 1, it is characterised in that: step In two, mixed phosphate used is that both sodium dihydrogen phosphate dihydrate and disodium hydrogen phosphate dodecahydrate are mixed with molar ratio 3:1 It closes.
4. the method that a kind of spray drying prepares Phosphation agar according to claim 1, it is characterised in that: step In two, the additive amount of mixed phosphate used is the 20 ~ 30% of agar powder material quality.
5. the method that a kind of spray drying prepares Phosphation agar according to claim 1, it is characterised in that: step In three, added catalyst is urea, and adding proportion is the 3 ~ 5% of agar powder material quality.
6. the method that a kind of spray drying prepares Phosphation agar according to claim 1, it is characterised in that: step In four, the solution ph is 5.5.
7. the method that a kind of spray drying prepares Phosphation agar according to claim 1, it is characterised in that: step It is 80 ~ 10rpm by the flow velocity that solution is sent into spray drying tower in five.
8. the method that a kind of spray drying prepares Phosphation agar according to claim 1, it is characterised in that: step In five, the inlet air temperature of spray drying tower is 140 ~ 165 DEG C, and atomisation pressure is 0.15 ~ 0.25MPa.
CN201810649172.XA 2018-06-22 2018-06-22 A kind of method that spray drying prepares Phosphation agar Pending CN108948228A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110003361A (en) * 2019-04-23 2019-07-12 绿新(福建)食品有限公司 A kind of preparation method of high-quality agar
CN110003362A (en) * 2019-04-23 2019-07-12 福建省绿麒食品胶体有限公司 A kind of preparation method of the modified agar of high grade of transparency high-gel strength
CN110482510A (en) * 2019-09-20 2019-11-22 瓮福达州化工有限责任公司 A kind of preparation process of food grade phosphoric acid hydrogen dipotassium
CN116375906A (en) * 2023-03-31 2023-07-04 集美大学 Preparation method of high-water-retention high-gel-strength agar

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003053565A1 (en) * 2001-12-21 2003-07-03 Muromachi Chemical Co., Ltd. Adsorbent for phosphoric acid
CN104498563A (en) * 2015-01-15 2015-04-08 福建省绿麒食品胶体有限公司 Gracilaria agaro-oligosaccharide and preparation method thereof
CN105642233A (en) * 2016-01-06 2016-06-08 河南工业大学 Method for preparing CMC/GO compound hydrogel microspheres by virtue of continuous method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003053565A1 (en) * 2001-12-21 2003-07-03 Muromachi Chemical Co., Ltd. Adsorbent for phosphoric acid
CN104498563A (en) * 2015-01-15 2015-04-08 福建省绿麒食品胶体有限公司 Gracilaria agaro-oligosaccharide and preparation method thereof
CN105642233A (en) * 2016-01-06 2016-06-08 河南工业大学 Method for preparing CMC/GO compound hydrogel microspheres by virtue of continuous method

Non-Patent Citations (1)

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何传波: "甘薯淀粉磷酸单酯制备机理及最优参数研究", 《中国优秀硕士论文全文数据库,工程科技Ⅰ辑,B024-5》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110003361A (en) * 2019-04-23 2019-07-12 绿新(福建)食品有限公司 A kind of preparation method of high-quality agar
CN110003362A (en) * 2019-04-23 2019-07-12 福建省绿麒食品胶体有限公司 A kind of preparation method of the modified agar of high grade of transparency high-gel strength
CN110482510A (en) * 2019-09-20 2019-11-22 瓮福达州化工有限责任公司 A kind of preparation process of food grade phosphoric acid hydrogen dipotassium
CN116375906A (en) * 2023-03-31 2023-07-04 集美大学 Preparation method of high-water-retention high-gel-strength agar

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