IP Library Granted Patent US 8,703,208
Granted Patent B2
US 8,703,208 · App. 12/403,904 · Granted Apr 22, 2014

Nanometer mesoporous silica-based xerogel styptic process and its preparing process and application

Inventors: Changsheng Liu (Shanghai, CN); Yuan Yuan (Shanghai, CN)
Assignee: East China University of Science and Technology
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Quick Facts
Patent No.
US 8,703,208
App. No.
12/403,904
Granted
Apr 22, 2014
Kind
B2
Abstract

The invention disclosed a novel mesoporous silica-based xerogel and its use in hemorrhage control. The mesoporous silica-based xerogel material has tunable mesopores (1-50 nm), high specific surface area (100-1400 m 2 /g), macroscopical morphology (powder, film, disc, column, etc.) and adjustable compositions (SiO 2 , CaO and P 2 O 5 , etc.) as well as good biodegradation. The mesoporous silica-based xerogels herein effectively promote the blood clotting under various conditions including slow and severe hemorrhage, even at the blood oozing site of bone defect. Meanwhile, the networks of silica-based xerogel with good elastic and mechanic properties, formed by adsorbing a large amount of water, can modulate the cell behavior and tissue growth, and thus promote the wound healing. Additionally, due to the mesoporous structure, the materials have the potential to load drug, thrombin and bioactive factors, which is favorable for the therapeutical efficacy.

Claims (25)

1. A mesoporous silica-based xerogel useful as a hemostatic material, comprising silicon oxide, calcium oxide and phosphor oxide at a molar ratio of about 50-100:5-20:5-20, the mesoporous silica-based xerogel has a porous structure that is amorphous, wherein the xerogel is obtained by a method consisting of:

dissolving a silica source precursor, a phosphorus source precursor and a calcium source precursor in an aqueous ethanol solution;

adjusting the pH of the obtained solution to a range of 2-8 using HCl, and stirring for about 1 to about 4 hours to obtain a stable sol;

aging the obtained sol at about 20 to about 100° C. for about 5 to about 200 hours, and then drying the sol; and

calcinating the dried sol at about 500 to about 700° C. for about 2 to about 10 hours to eliminate the solvent.

2. The mesoporous silica-based xerogel of claim 1 , wherein said mesoporous silica-based xerogel is biodegradable.

3. The mesoporous silica-based xerogel of claim 2 , wherein said mesoporous silica-based xerogel has an in vivo exothermic effect lower than that of zeolite.

4. The mesoporous silica-based xerogel of claim 3 , wherein when in vivo exothermic effect of the mesoporous silica-based xerogel is measured in the method as shown in example 6, the maximum temperature in the wounds treated is <42° C.

5. The mesoporous silica-based xerogel of claim 1 , wherein said mesoporous silica-based xerogel is biocompatible.

6. The mesoporous silica-based xerogel of claim 2 , wherein said mesoporous silica-based xerogel has a pore size ranging from 1 nm to 50 nm.

7. The mesoporous silica-based xerogel of claim 2 , wherein said mesoporous silica-based xerogel has a specific surface area of 100-1400 m 2 /g.

8. The mesoporous silica-based xerogel of claim 2 , wherein said mesoporous silica-based xerogel is in the form of powder, film, disc or column.

9. The mesoporous silica-based xerogel of claim 2 , wherein the xerogel further comprises antibiotics or thrombin.

10. A method for preparing the mesoporous silica-based xerogel according to claim 1 , wherein said method consisting of: dissolving a silica source precursor, a phosphorus source precursor and a calcium source precursor in an aqueous ethanol solution; adjusting the pH of the obtained solution to a range of 2-8 using HCl, and stirring for about 1 to about 4 hours to obtain a stable sol; aging the obtained sol at about 20 to about 100° C. for about 5 to about 200 hours, and then drying the sol; and calcinating the dried sol at about 500 to about 700° C. for about 2 to about 10 hours to eliminate the solvent.

11. The method of claim 10 , wherein the silica source is selected from the group consisting of tetraethoxysilane (TEOS), tetramethoxysilane (TMOS), tetrabutoxysilane (TBOS), sodium silicate, potassium silicate and lithium silicate.

12. The method of claim 10 , wherein the calcium source is selected from the group consisting of CaCl 2 , Ca(NO 3 ) 2 , (CH 3 COO) 2 Ca.H 2 O, methoxy calcium, ethoxy calcium and methoxyethoxy calcium.

13. The method of claim 10 , wherein the phosphorus source is selected from the group consisting of trimethyl phosphate (TMP), triethyl phosphate (TEP), Na 3 PO 4 , Na 2 HPO 4 , NaH 2 PO 4 , K 3 PO 4 , K 2 HPO 4 and KH 2 PO 4 .

14. The method of claim 10 , wherein the silica source, the phosphorus source and calcium are provided at a molar ratio of 50-100:0-25:0-25.

15. A method of hemostatic treatment, comprising the step of applying the mesoporous silica-based xerogels according to claim 1 to a bleeding site of the subject in need of to stop bleeding.

16. The method of claim 15 wherein the bleeding site includes slow and severe hemorrhage, inaccessible bleeding wounds, and blood oozing in bone defect.

17. The mesoporous silica-based xerogel of claim 4 , wherein the maximum temperature in the wounds treated is <40° C.

18. The mesoporous silica-based xerogel of claim 4 , wherein the maximum temperature in the wounds treated is <39.5° C.

19. The mesoporous silica-based xerogel of claim 1 , wherein the silica source is selected from the group consisting of tetraethoxysilane (TEOS), tetramethoxysilane (TMOS), tetrabutoxysilane (TBOS), sodium silicate, potassium silicate and lithium silicate.

20. The mesoporous silica-based xerogel of claim 1 , wherein the calcium source is selected from the group consisting of CaCl 2 , Ca(NO 3 ) 2 , (CH 3 COO) 2 Ca.H 2 O, methoxy calcium, ethoxy calcium and methoxyethoxy calcium.

21. The mesoporous silica-based xerogel of claim 1 , wherein the phosphorus source is selected from the group consisting of trimethyl phosphate (TMP), triethyl phosphate (TEP), Na 3 PO 4 , Na 2 HPO 4 , NaH 2 PO 4 , K 3 PO 4 , K 2 HPO 4 and KH 2 PO 4 .

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 18, 2024
From: SUZHOU BAIJI BIOTECH CO., LTD.
To: YIXIN BIO-TECH (GUANGZHOU) CO.,LTD
Reel/Frame 069382/0844 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 21, 2021
From: SHANGHAI YANKAI BIOTECH CENTER
To: SUZHOU BAIJI BIOTECH CO., LTD.
Reel/Frame 054990/0961 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 27, 2020
From: EAST CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
To: SHANGHAI YANKAI BIOTECH CENTER
Reel/Frame 054182/0104 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 29, 2009
From: LIU, CHANGSHENG; YUAN, YUAN
To: EAST CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
Reel/Frame 022754/0602 →
Priority Claims (1)
CN 2006 1 0116061 · Sep 14, 2006 · national
Continuity (2)
Continuation In Part PCTCN2006002907 · Oct 30, 2006
Related Publication 20090232902A1 · Sep 17, 2009